前苏联专利SU1075980A3 Fibrous mass

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专利摘要:
1491078 Cellulose fibre compositions MONSANTO CO 14 March 1975 [15 March 1974] 10654/75 Heading C3F A composition comprises discontinuous cellulose fibre, a thermoplastic polymer and a lubricant of molecular weight greater than 95. The polymer is present in a proportion of from 2% to up to half the weight of the cellulose. A wide variety of polymers are listed, but the exemplified ones are natural rubber, a copolymer of vinyl chloride and vinyl acetate, ethylenepropylene terpolymer and styrene-butadiene copolymer. The lubricant is absorbed by the fibre and increases its receptivity toward the polymer so that the polymer coats it; it is present in a proportion of from 5 to 60 parts by wt. per 100 parts of cellulose. A great number of materials is listed but the preferred are vegetable and mineral oils, paraffinic processing oil, aromatic processing oil diundecyl phthalate and liquid polybutene. The composition is intended to be used as a concentrate to be diluted by other materials to make up such things as moulding compositions. Other materials that may be added include carbon black, a bonding agent which may be alkylene resorcinol polymer plus hexamethoxymethylmelamine or an isocyanate bonding agent, zinc oxide, stearic acid, sulphur if the product is to be vulcanized, a sulphenamide, p - phenylenediamine, hexamethylenetetramine, TiO 2 and an organic ketene dimer. The cellulose fibre is preferably cotton, hardwood pulp or softwood pulp.
公开号:SU1075980A3
申请号:SU752117202
申请日:1975-03-14
公开日:1984-02-23
发明作者:Хамед Парвис
申请人:Монсанто Компани (Фирма)；
IPC主号:

专利说明:

-vj
SP
CO CX) The invention relates to rubber production, in particular to the development of pulp used as a filler for rubber compounds. Known fibrous mass (for filling rubbers J, including cellulosic staple fiber and lubricant plasticizing agent, for example, ester 11J. The resulting fibrous mass is characterized by unsatisfactory dispersion conditions, which leads to rubber with low physical and mechanical properties. The purpose of the invention is improving the distribution of the pulp in rubber mixtures. The goal is achieved by the fact that the pulp including cellulose staple fiber and plasticizing lubricant locator further comprises a polymer from the group you ranny natural rubber product of butadiene-styrene rubber, butadiene-iitrilny rubber, ethylene propylene terpolymer, butadiene-sti roll-vinylpyridine terpolymer, vinyl chloride-vinyl acetate copolymer, a mixture of PVC with nitrile-butadiene rubber in a ratio of 30:70 , chloroprene, in the following ratio of components, Macy.ch .: Cellulose staple fiber100 Specified polymer 5-6 Lubricant agent plasticizer 10-6 Examples 1-11. As an illustration of an example of compositions pre
Corn oil (MazOla)
1 2 3
Vegetable oil (v / esson)
Olive oil
Cottonseed Oil
four
Dry turpentine
five
Castor oil
b
Aromatic processing oil
7
Palm oil
eight
Peanut butter
9
Rosin oil
0 11
The rapeseed oil of the dispersed (treated) fiber, including both a plastic polymer and a lubricating agent, is shown in composition. qi based on wood fiber. hard rock that is treated with Omazy-. agent and mixed with natu-. solid (synthetic) rubber in a closed mixer. The treated filler (fibrous mass.) Is injected into a rubber mixture, pre / 1 part of a self-drying mixture, which is designated as U-1 H, 1 wt.h .: Natural rubber 5p, 0 Styrene-butadiene rubber50.0 Black soot furnace abrasion 50.0 Precipitated silica (Hi-Sil) 5.0 Zinc oxide3.0 p-Phenylenediamine agent against descrustation 2.0 Stearic acid 1.0 Concentrates (fibrous mass) fibers contain 5-60 wt.ch. rubber and 10-60 ma.ch. lubricating agent for every 100 ma.ch. the fibers. The masterbatch H-1 is mixed with the fibrous mass in a closed mixer for 5-10 minutes. Lubricating agents are identified in the table. .one. In these embodiments and in all subsequent embodiments, the amounts of all the products and the compositions of all the concentrates are expressed in mass parts for every 100 parts by weight of fiber, unless otherwise indicated. blitz 1 Lubricating agent
The content of the lubricating agent and rubber in examples 1-11, respectively: 1-20 and 20; 2 ..- 20 and 10 3-5 and 60; 4-10 and 30, "5-10 and 20; 6-40 and 10; 7-60 and 10; 8-50 and 10; 9-20 and 20; 10-30 and 20 and 11-10 and 15.
Each of the fiber concentrates is used to produce a fiber-reinforced polymer by mixing 102 parts by weight. concentrate (pulp) from 149 May, h. Royal mixture H-1, 5 MAH. methylene acceptor, 5 ma.ch. aromatic oil for polymer processing, 1 wt.h. methylene donor, 2 wt.h. sulfur and 1 wt.h. M-tert-butyl-2-benzothiazole sulfene-MID in a Banbury mixer for 6 minutes at low speed of rotation of the stirrer (77 rpm). After rolling into sheet material on rollers and curing for 30 minutes in a press at 152, (307 ° F), the tensile strength of each sample of complex material in the direction of the main fiber orientation (orientation 0 °) is equal to or greater than 140 kg / cm and the modulus of Young of such samples is equal to or exceeds 2109 kg / cm2, in all cases, extremely good and rapid dispersion of the fiber concentrate is observed.
On the basis of concentrates 7-11, complex materials are manufactured, the tensile strength of which is 175-, 210 kg / cm, and their Young's modulus exceeds 2109 kg / cm.
In addition, concentrates 8–11 provide pleasant smells to the final materials.
Example 12. As an illustration of another embodiment, 800 wt.h. ethylene-propylene terpolymer (EPDM rubber) with Mooney plasticity (1 - + - 4) at 121., equal to about 70, 6000 mash. of dry mass of hardwood 800 wt.h. furnace soot FEF and 1600 wt.h. paraffin oil. These components are mixed for about 5 minutes and discharged from the bottom of 9200 wt.h. Concentration for every 100 mah. fiber includes 13.3 wt.h. rubber and furnace soot and 26.6 wt.h. lubricating agent.
To illustrate the possibility of using this concentrate in a 1-A Banbury mixer with a capacity of approximately 16026 ml load
800 wt.h. EPDM rubber with plasticity ML 1 + 4) at 121.1 ° С approximately 7.0; 1000 parts by weight EPDM rubber with plasticity ML (1 + 4) at 121.1 ° C approximately 60.2200 parts by weight of stove FEF; 2300 parts by weight concentrate (example 12); 1600 wt.h. paraffin oil for polymer processing, 100 wt.h. zinc oxide; : 20 wt.h. stearic acid; 100 wt.h. alkylenresorcin binder agent, 40 wt.h. methylene donor (hexamethoxymethylmelamine) and 140 wt.h. vulcanizing agents. The components stirred the rotational speeds of the stirrer for 35 rpm for 6 minutes (the minimum duration required to disperse the treated fiber, as determined by visual observation) and unload, remove the complex material, which contains 75 wt.h. for every 100 wt.h. rubber
The total mixing time is calculated taking into account both the time required to prepare the pre-dipped fiber and the time needed to make the complex material from pre-dipped fiber. Since the time required to prepare the unit of a product determines the efficiency of obtaining only a part of the masterbatch used in the preparation of the final complex material, the time needed to prepare the specified part is used to calculate the total mixing time by multiplying the part used uterine concentrate for a 5 minute stirring time to prepare the total uterine concentrate with the addition of the time thus calculated nor by 6 minutes, which are required for mixing part of the concentrate. Parts of the composite material through rollers with equal speeds of rotation of the rolls in order to orient the fiber and give the composite material a molten shape. Oriented sheets are vulcanized to a press during the periods of time indicated in the rheometric data to achieve optimal vulcanization. The continuity of mixing and the physical properties of the vulcanized complex material; determined in the direction of the main orientation of the fiber (orientation O), are presented in Table. 2
Table 2
7.25
1879
12 The data show that a complex fiber-reinforced material with the desired physical properties is made in a short mixing cycle from a fiber pre-treated with a polymer combined with a lubricating agent. . Example 13 However, in another embodiment, using natural rubber and another lubricating agent, the load is 1000 m.h. natural rubber, 1000 wt.h. furnace black soot SPF, .1500 ma.h. lubricating agent 5000 MAH. dry weight of solid wood. These components are mixed for about 5 minutes and discharged to obtain 8500 wt.h. to the center (fibrous mass). As an illustration, it is possible to use this concentrate in a 0-0 Banbury mixer (with a capacity of approximately 4310 ml).
224
Dianodecyl phthalate
Examples 14-16. To illustrate the effect of the combination and the individual additives for treating the fiber, three concentrates are prepared by mixing the components listed in table. 4, in a Banbury B mixer at a speed of 14 component I 15 T 16
The mass of wood is firm
breeds
Styrene-butadiene copolymer rubber
Lubricant (aromatic oil for polymer processing)
Uterine volume factor
mixtures
Table 3
3480
155 about. / min
at
mixers
for 5 minutes
Also indicated is a masterbatch volume factor, which is the quantity by which the number of parts by mass should be multiplied to obtain
loadable quantities.
Table
Concentrate, parts by weight, example
: g
100
100
ten
30 7.0
8.0 900 ma.ch. peptized natural rubber, 850 wt. concentrate (from example 13), 300 mah. oven soot SPFj 50 ma.ch. precipitated silica, 500 mach. zinc oxide, 20 wt. stearic acid, 20 wt.h.p.-phenylenediamine agent that prevents the destruction, iSO wt.h. alkylenesouIdine binding agent, 20 wt.h. hexamethoxymethylamine, 20 mph. sulfur and 10 ma.ch. eulfenamide ukoritel. The components mix when rotating the agitator at 50 ppm / min for b min. You observe fast dispersion, as a result, you get a complex material containing 50 ma.h. fibers on 100 mach. rubber This complex material is oriented on rollers e the same. With a roll spinning and vulcanizing process, the optimum vulcanization is carried out. Physical properties are given in table. 3
Composite materials are prepared by diluting the concentrates indicated in Table. 4, in a Banbury B mixer at the speed of rotation of the mixer. 77 rpm for the time specified in table. 5. In each case, the initial mixture includes, m.ch .: 150 natural rubber; 150. furnace soot with high abrasion resistance; 22.5 silica; 9 zinc oxides; 3 stearic acid; bN-3 & ned p-phenylenediamine agent-. one that prevents destruction; 15 alkyleneresorcinol binder, agape-preventing degradation; 15 alkylene ether binding agent,
Styrene-butadiene copolymer rubber
Aromatic Oil for Polymer Processing
Concentrate 14

Concentrate 15 Concentrate 16 Mixing duration, min
Dispersing
These data indicate that complex material is prepared for a shorter period of time using fiber concentrate, treated with either a plastic poly, measure, or a lubricating agent, than using fiber treated only with either a polymer or a lubricating agent. Moreover, it is possible to conclude from the data on the determination of stress-strain using a vulcanization product with orientation O, that the Young's modulus of the initial mixture A is much higher than that of Young mixture of the initial mixture B or initial mixture C. In the case when it is desirable to reduce the moisture content to a minimum, vulcanizing agents can be eliminated and the treated fiber mixed with the base composition at a high speed of rotation of the agitator in a Banbury mixer. Created high temperate; 3 hexamethylenetetramine; b sulfur; 3 sulfenamide accelerator together with the variable components listed in the table. 4. The indicated time is the minimum duration required to disperse the fiber (as determined by visual means). So, for example, a visual observation of the initial mixtures B and C after bb min of mixing, which is enough to disperse the fiber of the initial mixture A7 shows that the fiber does not have enough time to disperse. The total weight of each initial mixture is 802.5 masses . h.
150
15
270
ten
Very good
tour provides effective removal of moisture. Then the mass is discharged and, after cooling, it is mixed with curatives and subjected to further desired processing.
Examples 17-20. Illustrated below are embodiments of the invention in which the concentrate is ready in t using rubber latex instead of mastic rubber.
In the Banbury mixer In load components that are listed in the table. 6 and they are mixed at a stirrer rotation speed of 155 rpm for approximately 2 minutes of loading the components and for 3 minutes after the plunger is lowered. An aqueous emulsion of styrene-butadiene-vinylpyridine terpoly is used as a latex: Measure containing 42% dry matter (the content of the elastomer is shown in parentheses).
Table 6
Voltage Characteristics
Strength at
gap, kg / cm2
Relative extension , %
Young's modulus,
kg / cm
Table 7 illustrates typical concentrates that contain 20 binding agents. Usually, concentrates containing binding agents are prepared in the same manner as described above, however, for the cases of using some coupling agents, it is necessary to perform special steps, allowing unregenerated cellulose fiber
Lubricating Agent Precipitated Silicon Dioxide Styrene-Butadiene Rubber
EPDA rubber (ethylene-propylene terpolymer)
Furnace carbon black FEF Binding agent
The treated fiber of Example 21 is a general purpose fiber that can be used to introduce into any elastomer with a high degree of unsaturation. The treated fiber of Example 22 is particularly suitable for mixing with low degree of unsaturation elastomers and is beneficial in applications where a high concentration of lubricant is acceptable in a reinforced complex material. The wood trail, obtained by the sulphate method, is a fiber that gives extremely high results in
Continued table. 7
263
267
232
4851
4534
3329
To achieve an appropriate degree of dispersion in the concentrate.
Examples 21-22. Alternatively, an initial mixture of rubber with a bonding agent can be prepared, followed by using this initial mixture to prepare a concentrate (Table 8).
Table 8
100
25-50
5-15 2-10 0.25-10
composition of any composition. Other suitable fibers are cotton fibers. These fibers are short threads of down, adhering to cotton seeds after the operation of cleaning the seed cotton. If desired, they can be replaced by the so-called cotton chemical varieties. For example, the composition 144.9 mph. the original U-1 H-1 masterbatch from 106.1 May; h. of chemical cotton concentrate and 5 parts by weight. Aromatic oil for nepepatSOTKH polymers is formed during half the time period that is required for the direct combination of components, while acquiring very good physical properties. The composition of such a concentrate 75 masosoch chemical cotton 15 ma.ch. aromatic oil for the processing of polymers and 16.1 wt. Royal mixture N-1. However, another suitable fiber is loose wood fiber. However, this fiber contains mainly lignin; It is produced by treating wood under the pressure of water vapor in an auto-clan, followed by relieving the pressure. The lubricant agent of example 21 is preferably selected from products of the aromatic type, which ensures its compatibility with styrene butyl rubber. Liquid novolac resins can be used as lubricants, which, in combination with hexamethylenetetramine or other bases, are added to the substrate to achieve good fiber bonding ability. Preferably the presence of silica. For use in conjunction with EPDM rubber of Example 22, an aliphatic type lubricating agent is desirable. Liquid polybutenes exhibit some of the characteristics of lubricating agents superior to those of petroleum-based lubricating oils used to lubricate metal surfaces - therefore they are also effective lubricating agents for fiber. The molecular weight of the polybutene lubricants is in the range of 400-2400. Chlorinated paraffin carbohydratesMass of dry wood Vinyl chloride copolymer
In each case, the fiber is carefully dispersed and ingibrated yarn-to-yarn agent. The treated fiber is easily mixed with polyvinyl chloride polymers to form compositions that can be used. in the most diverse applications of polyvinyl chloride. The addition of fiber in the form of a concentrate allows to obtain mixtures based on polyvinyl100
100
chloride, reinforced with fiber, which in other cases is associated with difficulties of technological order, or is impossible in general, depending on the availability of mixing means.
Cellulose fiber treated with a vinyl chloride polymer or copolymer resin and lubricant is particularly valuable for making plastic tiles for hydrogen and combining the wetting properties of the fiber with the ability to suppress flame spread, which is an advantage in some applications. As indicated above, the alkylene resorcinol binding agent can be replaced with other resorcinol based binding systems, some of which are resorma formaldehyde resins. In the process of obtaining mixtures of treated fiber, other methylene donors can be used in combination, in particular, dimethylol urea, dimethyl ethylene urea, and hexametoximethyl melamine. The isocyanate binding systems include: methylene-5c-phenyl-isocyanate, CH (methanol-5-phenyl-carbanilate NCO, CH (CbH4: INS- (0) -OCbH5.) 2, - 2,4-toluene diisocyanate,; three - (isocyanophenyl) methane, CH (C H4CHO) 2 and polymethylene polyphenylisocyanocideTo Usually isocyanates are used in the range of 0.252, 5 parts by weight, and resorcin-based resins in an amount of 3-10 parts by weight. Examples 23-25. Concentrates , described in Table 9, are prepared from a non-elastomeric polymer by loading it into an indoor mixer together with hardwood fiber, solid colivinyl chloride resin with a phthalate ester as a lubricant, and the components are mixed for 3. minutes at a stirrer speed of 155 rpm for heating the polymer to soften, heat is produced with water vapor. Table 9 floors, fiber-reinforced polyurethane resin, containing more than 50% polyvinyl chloride, is commonly used to make floor tiles, examples of which are copolymers with vinyl acetate or vinylidene chloride, with typical molecules th copolymer include vinyl chloride 87% vinyl acetate. The use of asbestos, which is the main reinforcing agent in the production of flooring tiles, requires special processing. Carrying out such a process requires a mass of asbestos fiber, solvents and a polymer, as well as a special type of calender necessary to eliminate the difficulties encountered when mixing and wetting the mass of asbestos fiber using PVC polymer with a high melt viscosity. Pre-dispersed cellulosic fiber can also be used as a reinforcing agent for such tiles, and it has been found that tiles containing cellulosic fibers have the ability to preserve better. ” dimensions, as well as a higher resistance to wear and abrasion than control plates containing asbestos fiber. The above-described pre-dispersion makes it possible to greatly simplify the manufacture of cellulose-fiber reinforced tiles. Moreover, the replacement of asbestos with pre-dispersed
Dry mass of solid wood
Lubricating agent
Butadiene-Acrylonitral Copolymer (Nusag 1052)
A mixture of butadiene-acrylonitrile copolymer with polyvinyl chloride 70/30 (Noosa g 1203)
Furnace soot FEF Neoprene CIS
The treated fiber is readily dispersed in plastic polymers combined with processing additives. So, for example, the concentrate at 5
100
100 16.6
20
ten
16.6
5 16,6
measure 27 is readily dispersed in the internal rubber during the 5-minute mixing cycle. A mixture of 110 May; .h. concentrate from 90 ma.h. This wood pulp requires the introduction of less fiber to achieve equivalent reinforcement. Adding organic ketene dimeric paper sizing agent improves water resistance. Organic ketene dimeric. Paper-gluing agents correspond to the general formula (to CH: C — O), where R is a hydrocarbon group, in particular alkyl, containing 8 or more carbon atoms, aryl. , aralkyl and alkaryl. Addition of 1% mixed hexadecyl-tetrade-; Cilketene dimer in terms of the weight of the fiber in the fiber concentrates of examples 23, 24 and 25 significantly improve the properties of tiles made on their basis. The amount of sizing agent is usually in the range of about 0.01-5% by weight, preferably 0.51% by weight, and this agent can be applied to silicon dioxide. Examples 26-28. Composition of other concentrates, illustrating examples prepared by treating the fiber with nitrile rubber with or without soot kiln, or with neoprene and furnace soot in a mixer for a 3-minute stirring cycle using phthalate ester as a lubricant also with nitrile rubber and aromatic oil for plastics processing as a lubricant agent, as well as with neoprene are presented in table. 10. Table 10
. butadiene copolymer and 30 ma.ch. reinforcing agent plus vulcanizing agents and binding components, after vulcanization in a press for 60 minutes at 152.8 ° C, gives a product of vulcanization, tensile strength — which in the direction of the main orientation of the fiber is 217 kg / cm and its Young's modulus is 3656 kg / cm
Equal parts of the neoprene concentrate of Example 28 and neoprene are easily mixed with each other, as well as with binding and vulcanizing agents with Formation after curing at 152, a vulcanization product whose tensile strength in the direction of the main orientation of the fiber is 221 kg / cm and the modulus Whose jung is equal to 3234 kg / cm2,.
In the examples of the practical embodiment of the invention, which are chosen for the purpose of illustrating it, any changes and modifications can be made without departing from the scope of the invention.
So, by virtue of the better distribution of fiber in rubber, the proposed fibrous mass in comparison with the known one is characterized by better physical and mechanical properties.

权利要求:
Claims (1)
[1]
FIBER MASS, including cellulosic staple fiber and a lubricating plasticizer, characterized in that, in order to improve the distribution of.-. lignin mass in rubber mixtures, it additionally contains a polymer selected from the group of natural rubber, styrene butadiene rubber, nitrile butadiene rubber, ethylene propylene terpolymer, styrene butadiene-vinyl pyridine terpolymer, vinyl chloride-vinyl acetate-polyvinyl butyryl nitride vinyl copolymer compound ratio of 30:70, chloroprene, in the following ratios of the components, wt.h .: cellulose staple fiber
Specified Polymer Lubricating Agent Fiber Catalyst
100
5-60
10-6Q g O

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同族专利:

公开号 | 公开日

NL178423C|1986-03-17|

IT1034290B|1979-09-10|

BR7501520A|1975-12-16|

AU7910975A|1976-09-16|

CS231156B2|1984-10-15|

LU72053A1|1976-02-04|

FR2264122A1|1975-10-10|

ZA751586B|1976-02-25|

CA1049712A|1979-03-06|

SE7502884L|1975-09-16|

SE427666B|1983-04-25|

GB1491078A|1977-11-09|

DE2511257C2|1983-06-01|

PL102238B1|1979-03-31|

AT381964B|1986-12-29|

PL107926B1|1980-03-31|

JPS5540620B2|1980-10-18|

JPS52141851A|1977-11-26|

US3943079A|1976-03-09|

FR2264122B1|1978-03-17|

JPS5754050B2|1982-11-16|

DE2511257A1|1975-09-18|

BE826686A|1975-09-15|

IN143844B|1978-02-11|

ATA197275A|1986-05-15|

SE7900915L|1979-02-02|

CS161875A2|1984-02-13|

ES449030A1|1977-07-01|

JPS50129637A|1975-10-14|

SE423105B|1982-04-13|

NL7502987A|1975-09-17|

AR213721A1|1979-03-15|

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法律状态:

优先权:

申请号 | 申请日 | 专利标题

US05/451,519|US3943079A|1974-03-15|1974-03-15|Discontinuous cellulose fiber treated with plastic polymer and lubricant|

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