• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    An absorbant for use in artificial organs which is obtained by mixing and dissolving pitch with an aromatic compound and a polymer or copolymer of a chain hydrocarbon, dispersing the resultant mixture in water giving rise to beads and subjecting these beads to a series of treatments of removing of the aromatic hydrocarbon, infusibilizing, carbonizing and activating.
    公开号:SU1088649A3
    申请号:SU792723052
    申请日:1979-02-06
    公开日:1984-04-23
    发明作者:Хино Куниаки；Уехара Ясуо；Нисимура Ясуси；Ватанабе Казухиро；Окада Есио
    申请人:Куреха Кагаку Когио Кабусики Кайся (Фирма)；
    IPC主号:
    专利说明:

    The invention relates to a method for producing a spherical carbon bioabsorbent and can be used in the medical field, for example, in artificial soil and the liver, etc., as well as in the food industry. A known method for producing a carbon adsorbent for hemodialysis involves the treatment of adsorbent granules, including activated carbon, with a solution of a copolymer containing carboxyl and amino groups in a solvent, for example dimethylformamide. The adsorbent with a polymer coating additionally applies a protein fume 13. The disadvantage of this method is that the polymer coating reduces the adsorption capacity of the resulting bioabsorbent, which prevents it from being used in clinical practice for artificial organs such as the liver and kidneys. The closest to the proposed technical essence and the achieved result is a method of obtaining a spherical bioabsorbent, including the formation of balls of molten resin - pitch - and an aromatic solvent by dispersion in aqueous solution, hardening and activation of the resulting balls, to remove dust, and applying a biocompatible polymer coating of albumin 23 on them. The disadvantage of this method is that the resulting adsorbent does not have sufficient strength due to its operation adsorbent releases coal dust during operation, which limits its use in artificial organs. The aim of the invention is to increase the strength of the bioabsorbent. The goal is achieved by the fact that C (5) according to the method for producing a spherical carbon bioabsorbent involving the molding of balls by dispersing a mixture of pitch and aromatic solvent in an aqueous solution, carbonizing and activating the extracted balls; and applying a biologically compatible coating, dispersing is carried out in the presence of a polymer, containing hydrocarbon chains, taken in an amount of 0.1-7.0% by weight of the mixture of pitch and aromatic solvent. At that, pec is used with a softening temperature of 201-225 With a carbon content of 94–95%, an hydrogen / carbon ratio of 0.54–0.61 and a nitrobenzene insoluble content of 21–37 wt.%. Moreover, benzene and naphthalene are used as an aromatic solvent. from the group comprising polyethylene, polypropylene, polybutadiene, polystyrene and ethylene-vinyl acetate copolymer. The method is carried out as follows: A resin with a softening point ranging from 201 to mixed with a compatible aromatic compound as a solvent and after melting and blending them with a friend, at temperatures ranging from 150 to them, a branched hydrocarbon polymer having a low degradability and a molecular weight of less than 500,000 is mixed for better blending with the mixture in the mixing temperature range in an amount of from 0.1 to 7% by weight of the mixture, followed by pouring the molten resinous mixture into water containing the suspending agent and maintained at a temperature in the range from 50 to, if necessary, in an autoclave, and dispersing the mixture in the form of spherical particles {balls |. Thereafter, the beads are processed to remove the aromatic compound used as an organic solvent in the molding process by extracting with a solvent in which the resin and polymeric material are not sufficiently soluble, but which exhibits good miscibility with the added bounded solvent. susceptible to curing, carbonization, activating and hardening in the usual way. Curing treatment is carried out on. air, gradually heating the product from room temperature, and complete at a temperature below 400 ° C. The solidified spherical resin is then heated and carbonized under N2 or steam and activated at 9001000 ° C. As a result of this, a spherical, low-dusting, high-strength activated carbon is obtained. In the preferred embodiment, the resin used as one of the components of the starting material has a softening point of 201-225 ° C, a carbon content of 9.4-95 wt.%, A hydrogen / carbon atomic ratio of 0.54-0.61, and a nitrobenzene content of insoluble matter 21 -37 wt.%. The term “softening point” is used to denote the temperature at which the piston of an instrument of the KOKA flow tester type, filled with 1 g of sample, comes to a first stop during the period of reduced movement that occurs after heating the sample at a temperature increasing at a rate of 6 C / min, with a load of 10 kg / cm. Under the term, the content of nitrobenzo-insoluble substance is understood as the ratio in mass percent of the insoluble substance remaining after adding 1 g of resin powder to 100 ml of nitrobenzene and astvoreni at 4Q ° C. Usually, any resin is applied with equal success, both from oil cracking and from coal. The adsorbent balls thus obtained are true spheres with the following physical properties: particle diameter from 0.1 to 1.5 MM} particle density from 0.5 to 1.5 G / ML} specific surface area from 800 to 1600 m2 / g; not less than 0.3 ml / pore volume has a pore radius of 100 A measured and less than 0.5 ml / g of pore volume has a pore radius in the range from 100 to 100,000 A. The ash content of the adsorbent is less than 0.5 wt. .%. The adsorption of a biocompatible substance by adsorbent balls is carried out by immersing them in an aqueous solution of a biological substance (blood component), such as albumin or heparin, removing the wet balls from the solution and drying them. When using a carbon adsorbent on which a biological component is applied, as an adsorbent in an artificially organ, blood is forced to flow through the adsorbent, while the blood and the biological component are deposited on the adsorbent and are kept in equilibrium near the surface of the balls. Example. The starting batch is obtained by spraying Ceria crude oil in steam at 2000 ° C with contact time of 0.005 s followed by thermal cracking of crude oil, rapidly cooling the oil thus subjected to cracking, rectification of the resinous material obtained in this way, and collecting fractions distilled at temperatures below, which at ordinary temperatures harden in the form of a pitch. The pitch thus obtained is characterized by a softening temperature of 201 ° C, a content of 37% insoluble nitrobenzene suspension, a carbon content of 95% by weight, and an atomic hydrogen / carbon ratio of 0.54, and is used to produce activated carbon. D autoclave per 1 liter of mix: wg of pitch obtained in this way, 100 g of naphthalene and polymer materials, such as polyethylene, polypropylene, polybutadiene, polystyrene, ethylene vinyl acetate copolymer in an amount of from 0.1 to 7% by weight of pitch, and the mixture is melted or fluidized with stirring and heating for 2 hours. The molten mixture is poured into hot water containing 0.5% by weight of polyvinyl alcohol while in another autoclave with stirring, and dispersed in the solution by further stirring at 1200 rpm within 20 min to transform Into spherical particles, after which the system is cooled to form solid spherical particles of a pitch mixture. After collecting the particles by filtration and dehydrating the particles, naphthalene from the particles is removed by extraction with n-hexane. The particles treated in this way are transferred to a fluidized state, while simultaneously heating them from room temperature to 300 ° C with the heating rate of AER / h to obtain non-melting particles. Thereafter, the non-melting particles are heated to a gas mixture consisting of 50% by volume nitrogen, 47% by volume water vapor and 3% by volume oxygen for conversion of activated carbon into spherical particles (hereinafter referred to as activated carbon). 100 g of the obtained beads are dispersed in 500 ml of distilled water. Dispersed balls are washed in an ultrasonic washer using ultrasonic vibrations for 30 minutes, then placed on a stainless steel mesh and washed with running water. The washed pillows are dispersed in 200 ml of ethanol-water mixture (80-20) containing 0, 1 wt.% Polyhydroxyethylmethacrylate. 800 ml of distilled water was carefully added to the dispersion to isolate the polyhydroxyethylmethacrylate as an independent phase to effect the first coating of the polyhydroxyethylmethacrylate beads. The coated beads are placed on stainless steel meshes, washed with distilled water to remove excess coating material and dried to obtain dust-free beads coated with polyhydroxyethyl methacrylate. EXAMPLE 2 By rectification of the bottom residue of ethylene production to remove fractions boiling below 1540 ° C, a residual product is obtained with a softening temperature of 225 ° C, a content of 21% by weight insoluble in nitrobenzene, a carbon content of 94% by weight and an atomic hydrogen / carbon ratio of 0.61, and this product is used as a starting pitch. In a 1 l autoclave, ZOOg of the resulting lek is mixed, 100 g of benzene and 9 g (30 by weight of polyethylene pitch, and the whole is heated for 2 hours with stirring to obtain a molten or liquefied mixture. This mixture is poured into hot water containing 0.5 wt.% polyvinyl alcohol at 170 ° C in another autoclave with stirring, is dispersed into the solution with continuous stirring for 20 minutes at 1200 rpm to turn into spherical particles, followed by cooling the system to obtain solid spherical particles mixes. While collecting particles by filtration and dehydrating the collected particles, the benzene particles are removed by n-hectane extraction. The particles thus obtained are transferred to a fluidized state while heating them from room temperature to 300 ° with a heating rate of 30 ° C per hour non-melting particles. After that, the non-melting particles are treated as in Example 1 to convert the activated carbon into spherical particles. In 500 ml of distilled water, 100 g of the balls obtained in Example 2 are dispersed. iki washed with ultrasonic waves for 30 mi in an ultrasonic washer, using correctly in Example 1. They were placed on a stainless steel .setku and washing with running water dissolved. This product is immersed in an aqueous 15% albumin solution and held for about 2 hours to adsorb the albumin. Balls are separated by draining an aqueous solution of albumin, and then drying, and getting albumin-treated Vb-containing beads. Prize (Comparative 1. To 500 ml of distilled water add 100 balls of activated carbon obtained by a known method. Balls in water are washed in an ultrasonic sonic washer for 30 minutes and separated from the washing liquid. Then they are again placed in 500 ml fresh distilled water and subjected to the same rinsing procedure. Then it is subjected to the third rinsing. After the third solution has been removed, remove the clean balls from activated carbon in running water. The balls purified in this way were not completely free from coal dust and subsequently covered with polyhydroxyethylmethacrylate film by the method indicated in Example 1. The ability of the floor: adsorbent to release dust was determined as follows: a; 10 g of the sample and 50 ml of distilled water were placed in a glass vessel with a diameter of 60 MI and 80 mm high and shaken with an amplitude of 40 mm at 250 rpm for 30 minutes, the resulting suspension is passed (to filter I through a strainer, 100 mesh. and washed with fresh distilled water. The filtrate is evaporated to dryness, after which the amount of the obtained fine nopoiuKtaj is measured. B) 5 g of the sample are placed in a 200 ml Erlenmeyra flask and 50 ml of distilled water is added to it. After degassing, the flask is hermetically sealed and shaken in the same manner as in the case of tx. Immediately after agitation, a sample of the supernatant liquid is taken to measure the transmission coefficient of the light using a spectrophotometer using a wavelength of 660 nm. The strength of the adsorbent is determined according to standard 3 / S-K-1474. The results of testing the ability to form dust, strength and other characteristics of the adsorbent according to the proposed and well-known methods are given in the table. Tests of the resulting adsorbent On the adsorption of various substances with different pH1 molecules (urea, uric acid, creatanine, vitmin insulin) showed that a biocompatible coating on the balls leads only to a slight decrease in the adsorbent capacity of the balls, containing five units of heparin, it was found that there was no adhesion to the bullets of blood platelets and corpuscles.
    Adsorption of iodine, mg / g. Discoloration of caramel. Apparently with density, to / cm
    l
    Specific surface, m / g
    Dusting ability
    Strength
    1080
    980 92
    1030 80
    0.45
    0.56
    Oh, 5 a
    1150
    1150 950
    e4, 7
    OD8 ena 84.1 95.2
    99.0
    权利要求:
    Claims (4)
    [1]
    1. A METHOD FOR PRODUCING A SPHERICAL CARBON BIOADSORBENT, comprising forming balls by dispersing a molten pitch and aromatic solvent mixture into an aqueous solution, carbonizing and activating the extracted balls, followed by applying a biocompatible coating to the balls, characterized in that, in order to increase the bio-adsorbent strength, in the presence of a polymer containing hydrocarbon chains, taken in an amount of 0.1-7.0% by weight of a mixture of pitch and aromatic solvent.
    [2]
    2. The method according to p. 1, about t l and ch. I mean that they use pitch with a softening temperature of 201-225 ° C, a carbon content of 94-95 wt.%, an atomic ratio of hydrogen / carbon of 0.54-0.61 and a content of fraction 21- insoluble in nitrobenzene
    [3]
    3 May 7.%. Ts
    3. ‘Pop. 1, it is distinguished by the fact that benzene and naphthalene are taken as the aromatic solvent.
    [4]
    4. The method according to π. 1, characterized in that the polymer is selected from the group consisting of polyethylene, polypropylene, polybutadiene, polystyrene, ethylene vinyl acetate copolymer.
    SU „<1088649 A
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    同族专利:
    公开号 | 公开日
    US4221695A|1980-09-09|
    NL7900894A|1979-08-08|
    DE2904430A1|1979-08-09|
    GB2017068B|1982-08-18|
    DE2904430C2|1983-05-11|
    BR7900716A|1979-09-04|
    GB2017068A|1979-10-03|
    IT1110254B|1985-12-23|
    ES477363A1|1980-07-01|
    NL178227C|1986-02-17|
    FR2416040B1|1983-07-29|
    JPS54105897A|1979-08-20|
    CA1108108A|1981-09-01|
    FR2416040A1|1979-08-31|
    JPS639869B2|1988-03-02|
    IT7919928D0|1979-02-06|
    引用文献:
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    JP53012140A|JPS639869B2|1978-02-06|1978-02-06|
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