一种含有动物毛发蛋白质的合成纤维及其制造方法 技术领域 Synthetic fiber containing animal hair protein and manufacturing method thereof
本发明涉及纺织领域, 尤其涉及一种含有从动物毛发中提取的蛋白质的 合成纤维, 本发明还提供了这种合成纤维的制造方法。 背景技术 The present invention relates to the field of textiles, and more particularly to a synthetic fiber containing proteins extracted from animal hair, and a method of producing such a synthetic fiber. Background technique
在申请号为 91109153. X的专利申请中, 公开了一种以高聚物为芯, 蛹蛋 白为外层的复合纤维, 本发明人又在专利号为 99116636. 1的专利中公开了一 种植物蛋白质合成纤维及其制造方法, 这为纤维生产扩大了资源。 目前, 申 请号为 02115722. 7的专利申请又公开了一种动物毛蛋白质再生纤维纺丝原液 及其制造方法, 这为生产纤维扩大了原料范围, 还可以把废物回收再利用, 但该发明申请仅仅公开了一种纺丝原液, 原液中动物毛蛋白质占 25-40份, 由于动物毛蛋白质中胱氨酸含量较大, 而胱氨酸的稳定性较差, 因此要把这 种纺丝原液制成纤维还需要有恰当的纺丝工艺与之配合, 并且这种原液制造 出的纤维的用途单一, 且强度差。 发明内容 In the patent application No. 91109153. X, a composite fiber having a core as a core and a ruthenium protein as an outer layer is disclosed, and the inventors disclose a patent in the patent No. 99116636. Plant protein synthetic fibers and methods for their manufacture, which expand resources for fiber production. At present, the patent application No. 02115722. 7 discloses an animal hair protein regenerated fiber spinning dope and a manufacturing method thereof, which expands the raw material range for producing fibers, and can also recycle waste, but the invention application Only one spinning dope is disclosed, and the animal hair protein in the original liquid accounts for 25-40 parts. Since the cystine content of the animal hair protein is large, and the stability of cystine is poor, the spinning dope is required. The fiber is also required to have a proper spinning process to match it, and the fiber produced by the stock solution has a single use and is inferior in strength. Summary of the invention
本发明的目的是提供用途更广泛的含动物毛发蛋白质的纤维, 并提供其 制造方法。 SUMMARY OF THE INVENTION An object of the present invention is to provide a fiber for animal hair protein containing a wider range of uses and to provide a method for producing the same.
本发明的目的是采用以下技术方案实现的: 一种含有动物毛发蛋白质的 合成纤维, 由蛋白质和聚乙烯醇组成, 所述的蛋白质为从由动物毛发中提取 的分离蛋白质, 纤维中蛋白质的含量为 1%到小于 25%或者从大于 40%到 90%。 The object of the present invention is achieved by the following technical solutions: A synthetic fiber containing animal hair protein, consisting of protein and polyvinyl alcohol, the protein is isolated protein extracted from animal hair, and the protein content in the fiber It is from 1% to less than 25% or from more than 40% to 90%.
所述的纤维中蛋白质的含量为 3% - 20%。 The fiber has a protein content of 3% to 20%.
所述的纤维中蛋白质的含量为 45%-90%。
制造所述的合成纤维的方法是: The protein has a protein content of 45% to 90%. The method of making the synthetic fiber is:
先从动物毛发中提取分离蛋白质; First extracting the isolated protein from animal hair;
再将分离蛋白质溶于含有十二烷基磺酸钠或三乙醇胺的水溶液中, 溶解 温度为 15 °C-95 °C , 溶解时间为 1. 5-4小时, 制成蛋白质溶液; Further, the isolated protein is dissolved in an aqueous solution containing sodium dodecyl sulfate or triethanolamine, the dissolution temperature is 15 ° C - 95 ° C, and the dissolution time is 1. 5 - 4 hours to prepare a protein solution;
而后把经水洗的聚乙烯醇直接加入蛋白质溶液中, 在 60Ό- 98°C的温度 下, 使它们共混共聚, 时间 1. 5-4 小时, 制得含蛋白质和聚乙烯醇的浓度为 8%- 14%或者 15%-38%的纺丝溶液; Then, the water-washed polyvinyl alcohol is directly added to the protein solution, and they are blended and copolymerized at a temperature of 60 Torr to 98 ° C for a period of 1.5 to 4 hours, and the concentration of the protein-containing and polyvinyl alcohol is 8 %- 14% or 15%-38% spinning solution;
向纺丝溶液中加入硼酸或硼 、调整粘度, 制成纺丝原液; Add boric acid or boron to the spinning solution, adjust the viscosity, and prepare a spinning dope;
紡丝原液在温度 50- 80° ( 、常压下静置脱泡 3-8小时,或在温度 30- 40°C、 真空静置脱泡 3-8小时, 进入纺丝程序, 制成蛋白质合成纤维。 Spinning stock solution at a temperature of 50-80 ° (at room temperature, defoaming for 3-8 hours, or at a temperature of 30-40 ° C, vacuum degassing for 3-8 hours, into the spinning process, made into protein Synthetic fiber.
从动物毛发中提取蛋白质时, 应将动物毛发去脂去杂后浸入酸性溶液中, 温度 20-90°C , 时间 1 - 8小时, 分离提纯除去废渣, 用碱调浸出液的等电点, 提取分离蛋白质。 When extracting protein from animal hair, the animal hair should be degreased and then immersed in an acidic solution at a temperature of 20-90 ° C for 1-8 hours. Separate and purify the waste residue, adjust the isoelectric point of the leachate with alkali, and extract. Protein is separated.
进入纺丝程序后, 可采用湿法纺丝工艺制成蛋白质合成纤维。 After entering the spinning process, the protein synthetic fiber can be formed by a wet spinning process.
纺丝溶液中含蛋白质和聚乙烯醇的浓度为 15%-38 , 进入纺丝程序后, 也 可采用干喷湿纺的纺丝工艺制成蛋白质合成纤维。 The concentration of protein and polyvinyl alcohol in the spinning solution is 15% to 38. After the spinning process, the protein synthetic fiber can also be produced by a dry-jet wet spinning process.
纺丝溶液中含蛋白质和聚乙浠醇的浓度为 20%- 38%, 进入纺丝程序后, 也 可采用干法纺丝工艺制成蛋白质合成纤维。 The concentration of protein and polyethylene glycol in the spinning solution is 20% to 38%. After the spinning process, the dry spinning process can also be used to form the protein synthetic fiber.
本发明不仅将动物的毛作为制造蛋白质的原料, 而且把人的碎头发也作 为制造蛋白质的原料, 这进一步扩大了制造纤维的原料来源, 使废物得以充 分利用。 本发明中的纤维, 当蛋白质的含量较低时, 由于聚乙烯醇含量较高, 且避免了 SH基氣基酸的不稳定性, 因此使所生产的纤维不仅具有弹性、 吸湿 性、 透气性好的特点, 而且强度好, 可以纺制成更细的纤维, 使织物更柔软。 当蛋白质的含量较高时, 制成的纤维弹性和亲肤性更好, 这种纤维具有天然 麻纤维的透爽性, 不仅穿着舒适, 而且是制造人造假发的极好材料, 所以本
发明为资源的利用开辟了更广泛的途径。 本发明在制纺丝液时是将分离蛋白 质溶于接近中性的三乙醇胺或十二梡基磺酸钠水溶液中, 聚乙烯醇又直接加 入该蛋白质溶液中, 因此制成的纤维不含不必要的无机化学成份, 且制造过 程中也不会对环境产生污染。 具体实施方式 The present invention not only uses animal hair as a raw material for producing protein, but also uses human broken hair as a raw material for producing protein, which further expands the source of raw materials for fiber production and makes full use of waste. In the fiber of the present invention, when the content of the protein is low, since the polyvinyl alcohol content is high, and the instability of the SH-based gas-based acid is avoided, the produced fiber is not only elastic, hygroscopic, and gas permeable. Good characteristics, and good strength, can be spun into finer fibers to make the fabric softer. When the protein content is high, the fiber is made to have better elasticity and skin-friendly properties. This fiber has the natural hemp fiber permeability, is not only comfortable to wear, but also an excellent material for making artificial wigs. Inventions have opened up a broader avenue for the use of resources. When the spinning solution is prepared, the separated protein is dissolved in the near-neutral aqueous solution of triethanolamine or sodium dodecylsulfonate, and the polyvinyl alcohol is directly added to the protein solution, so that the produced fiber does not contain no Necessary inorganic chemical composition, and no pollution to the environment during the manufacturing process. detailed description
实施例 1: 将动物毛去脂去杂后浸泡在 PH为 1. 5的水溶液中, 并进行搅 拌, 在温度 70Γ经过 6小时后分离提纯除去废渣, 用碱调浸出液的等电点, 得分离蛋白质; 将分离蛋白质溶于含有十二烷基磺酸钠的软水溶液中, 溶解 温度为 15 °C , 溶解时间为 4小时, 制成蛋白质溶液; 将一定量水洗纯净的聚 乙烯醇直接加入蛋白质溶液中, 使它们共混共聚, 其温度緩慢升至 98 °C, 保 持 1. 5小时, 其间加入软水调节浓度, 制得含蛋白质和聚乙烯醇的浓度为 14% 的纺丝溶液, 其中蛋白质和聚乙烯醇的干固量重量比为 3 : 97; 向纺丝溶液中 加入硼酸调整粘度, 制成纺丝原液; 纺丝原液在温度 30°C , 真空条件下静置 脱泡 8小时, 进入纺丝程序, 用湿法纺丝工艺制成蛋白质合成纤维。 Example 1: The animal hair was degreased and then immersed in an aqueous solution having a pH of 1.5, and stirred. After 6 hours at a temperature of 70 Torr, the separation and purification were carried out to remove the waste residue, and the isoelectric point of the leaching solution was adjusted with a base to obtain a separation. Protein; the isolated protein is dissolved in a soft aqueous solution containing sodium dodecyl sulfate, the dissolution temperature is 15 ° C, the dissolution time is 4 hours, and the protein solution is prepared; a certain amount of washed pure polyvinyl alcohol is directly added to the protein. In the solution, they were blended and copolymerized, and the temperature was slowly raised to 98 ° C for 1.5 hours, during which soft water was added to adjust the concentration to obtain a spinning solution containing protein and polyvinyl alcohol at a concentration of 14%, wherein the protein The weight ratio of dry solid to polyvinyl alcohol is 3:97; the boric acid is added to the spinning solution to adjust the viscosity to prepare a spinning dope; the spinning dope is degassed under vacuum for 8 hours at a temperature of 30 ° C. Into the spinning process, a protein synthetic fiber is produced by a wet spinning process.
实施例 2: 将动物毛去脂去杂后浸泡在 PH为 2的水溶液中, 并进行搅拌, 在温度 40°C经过 7小时后分离提纯除去废渣, 用碱调浸出液的等电点, 得分 离蛋白质; 将分离蛋白质溶于含有十二浣基磺酸钠的软水溶液中, 溶解温度 为 30°C , 溶解时间为 2小时, 制成蛋白质溶液; 将一定量水洗纯净的聚乙烯 醇直接加入蛋白^溶液中,使它们共混共聚,其温度緩慢升至 98 °C ,保持 3. 5 小时,其间加入软水调节浓度, 制得含蛋白质和聚乙烯醇的浓度为 27%的紡丝 溶液, 其中蛋白盾和聚乙烯醇的干固量重量比为 60: 40; 向纺丝溶液中加入 硼酸调整粘度, 制成纺丝原液; 纺丝原液在温度 4 G°C、 真空条件下静置脱泡 4小时, 进入纺丝程序, 用湿法纺丝工艺制成蛋白质合成纤维。 Example 2: The animal hair was degreased and then immersed in an aqueous solution of pH 2, and stirred. After 7 hours at a temperature of 40 ° C, the separation and purification were carried out to remove the waste residue, and the isoelectric point of the leachate was adjusted with a base to obtain a separation. Protein; the isolated protein is dissolved in a soft aqueous solution containing sodium dodecyl sulfonate, the dissolution temperature is 30 ° C, the dissolution time is 2 hours, and the protein solution is prepared; a certain amount of washed pure polyvinyl alcohol is directly added to the protein ^ In the solution, they were blended and copolymerized, and the temperature was slowly raised to 98 ° C for 3.5 hours, during which soft water was added to adjust the concentration to obtain a spinning solution containing protein and polyvinyl alcohol at a concentration of 27%, wherein The dry weight ratio of protein shield and polyvinyl alcohol is 60: 40; boric acid is added to the spinning solution to adjust the viscosity to make a spinning dope; the spinning dope is allowed to defoam at a temperature of 4 G ° C under vacuum. After 4 hours, the spinning process was carried out, and the protein synthetic fiber was prepared by a wet spinning process.
实施例 3: 将人发去脂去杂后浸泡在 PH为 2. 3的水溶液中, 并进行搅拌,
在温度 90°C经过 4小时后分离提纯除去废渣, 用碱调浸出液的等电点, 得人 发分离蛋白质; 将分离蛋白质溶于含有十二烷基磺酸钠的软水溶液中, 溶解 温度为 60。C, 溶解时间为 1. 5小时, 制成蛋白质溶液; 将一定量水洗纯净的 聚乙烯醇直接加入蛋白质溶液中, 使它们共混共聚, 其温度緩慢升至 98 °C , 保持 2. 5 小时, 其间加入软水调节浓度, 制得含蛋白质和聚乙烯醇的浓度为 38%的纺丝溶液, 其中蛋白质和聚乙烯醇的干固量重量比为 45: 55; 向纺丝溶 液中加入硼酸调整粘度, 制成纺丝原液; 纺丝原液在温度 35 °C、 真空条件下 静置脱泡 3小时, 进入纺丝程序, 用湿法纺丝工艺制成蛋白盾合成纤维。 Example 3: The human hair is degreased and then immersed in an aqueous solution having a pH of 2.3, and stirred. After 4 hours at a temperature of 90 ° C, the separation and purification are carried out to remove the waste residue, and the isoelectric point of the leaching solution is adjusted with a base to obtain a protein for human hair separation; the separated protein is dissolved in a soft aqueous solution containing sodium dodecyl sulfate, and the dissolution temperature is 60. 5小时。 The temperature is slowly increased to 98 ° C, maintaining 2. 5 hours, the temperature is slowly increased to 98 ° C, the temperature is slowly increased to 98 ° C, kept for 2.5 hours , adding soft water to adjust the concentration, to obtain a spinning solution containing 38% of protein and polyvinyl alcohol, wherein the dry weight ratio of protein to polyvinyl alcohol is 45: 55; adding boric acid to the spinning solution The viscosity is made into a spinning dope; the spinning dope is degassed at a temperature of 35 ° C under vacuum for 3 hours, and enters a spinning process to form a protein shield synthetic fiber by a wet spinning process.
实施例 4: 将动物毛和人发去脂去杂后, 一起浸泡在 PH为 2. 6的水溶液 中, 并进行搅拌, 在温度 20°C经过 8小时后分离提纯除去废渣, 用碱调浸出 液的等电点, 得分离蛋白质; 将分离蛋白质溶于含有十二烷基磺酸钠的软水 溶液中, 溶解温度为 50Ό , 溶解时间为 3. 8小时, 制成蛋白质溶液; 将一定 量水洗纯净的聚乙烯醇直接加入蛋白质溶液中, 使它们共混共聚, 其温度緩 慢升至 98 °C , 保持 4小时, 其间加入软水调节浓度, 制得含蛋白质和聚乙烯 醇的浓度为 8%的纺丝溶液, 其中蛋白质和聚乙烯醇的干固量重量比为 1: 99; 向纺丝溶液中加入硼酸调整粘度, 制成纺丝原液; 纺丝原液在温度 38°C、 真 空条件下静置脱泡 5. 5 小时, 进入纺丝程序, 用湿法纺丝工艺制成蛋白质合 成纤维。 Example 4: The animal hair and the human hair were degreased, and then immersed in an aqueous solution having a pH of 2.6 and stirred. After 8 hours at a temperature of 20 ° C, the separation and purification were carried out to remove the residue, and the leaching solution was adjusted with a base. The isoelectric point, the protein is separated; the separated protein is dissolved in a soft aqueous solution containing sodium dodecyl sulfate, the dissolution temperature is 50 Ό, the dissolution time is 3.8 hours, and the protein solution is prepared; The polyvinyl alcohol was directly added to the protein solution, and they were blended and copolymerized. The temperature was slowly raised to 98 ° C for 4 hours, and soft water was added thereto to adjust the concentration to obtain a protein-containing and polyvinyl alcohol concentration of 8%. a silk solution, wherein the dry weight ratio of protein to polyvinyl alcohol is 1:99; boric acid is added to the spinning solution to adjust the viscosity to prepare a spinning dope; the spinning dope is allowed to stand at a temperature of 38 ° C under vacuum After defoaming for 5. 5 hours, the spinning process was carried out, and the protein synthetic fiber was prepared by a wet spinning process.
实施例 5: 将动物毛去脂去杂后浸泡在 PH为 3的水溶液中, 并进行搅拌, 在温度 98 °C经过 1小时后分离提纯除去废渣, 用碱调浸出液的等电点, 得分 离蛋白盾; 将分离蛋白质溶于含有三乙醇胺的软水溶液中, 溶解温度为 25 °C , 溶解时间为 3. 5 小时, 制成蛋白质溶液; 将一定量水洗纯净的聚乙烯醇直接 加入蛋白质溶液中, 使它们共混共聚, 其温度緩慢升至 98 °C, 保持 2小时, 其间加入软水调节浓度, 制得含蛋白质和聚乙烯醇的浓度为 33%的纺丝溶液, 其中蛋白质和聚乙烯醇的干固量重量比为 20: 80; 向纺丝溶液中加入硼砂调
整粘度, 制成纺丝原液; 纺丝原液在温度 50°C、 常压下静置脱泡 7小时, 进 入紡丝程序, 用湿法纺丝工艺制成蛋白质合成纤维。 Example 5: The animal hair was degreased and then immersed in an aqueous solution of pH 3, and stirred. After 1 hour at a temperature of 98 ° C, the separation and purification were carried out to remove the waste residue, and the isoelectric point of the leachate was adjusted with a base to obtain a separation. Protein Shield; The isolated protein is dissolved in a soft aqueous solution containing triethanolamine, the dissolution temperature is 25 ° C, the dissolution time is 3.5 hours, and the protein solution is prepared; a certain amount of washed pure polyvinyl alcohol is directly added to the protein solution. , they were blended and copolymerized, and the temperature was slowly raised to 98 ° C for 2 hours, during which soft water was added to adjust the concentration to obtain a spinning solution containing 33% of protein and polyvinyl alcohol, in which protein and polyvinyl alcohol were used. The dry solid weight ratio is 20: 80; adding borax to the spinning solution The final viscosity is made into a spinning dope; the spinning dope is allowed to defoam for 7 hours at a temperature of 50 ° C under normal pressure, and is subjected to a spinning process to form a protein synthetic fiber by a wet spinning process.
实施例 6: 将动物毛去脂去杂后浸泡在 PH为 1. 1的水溶液中, 并进行搅 拌, 在温度 30°C经过 5小时后分离提纯除去废渣, 用碱调浸出液的等电点, 得分离蛋白质; 将分离蛋白盾溶于含有三乙醇胺的软水溶液中, 溶解温度为 75 °C , 溶解时间为 2. 5 小时, 制成蛋白质溶液; 将一定量水洗純净的聚乙烯 醇直接加入蛋白质溶液中,使它们共混共聚,其温度緩慢升至 98 °C ,保持 1. 8 小时, 其间加入软水调节浓度, 制得含蛋白质和聚乙烯醇的浓度为 20%的纺丝 溶液, 其中蛋白盾和聚乙烯醇的千固量重量比为 40 : 60; 向纺丝溶液中加入 硼^ H周整粘度, 制成纺丝原液; 纺丝原液在温度 80° (:、 常压下静置脱泡 5小 时, 进入纺丝程序, 用湿法纺丝工艺制成蛋白质合成纤维。 Example 6: The animal hair was degreased and then immersed in an aqueous solution having a pH of 1.1, and stirred. After 5 hours at a temperature of 30 ° C, the separation and purification were carried out to remove the waste residue, and the isoelectric point of the leachate was adjusted with a base. We have isolated protein; separating the aqueous solution containing the protein soft shield dissolved triethanolamine, dissolution temperature of 75 ° C, the dissolution time being 25 hours to prepare a protein solution; the amount of pure water was added directly to the polyvinyl alcohol In the protein solution, they were blended and copolymerized, and the temperature was slowly raised to 98 ° C for 1.8 hours, during which soft water was added to adjust the concentration to obtain a spinning solution containing protein and polyvinyl alcohol at a concentration of 20%. The weight ratio of protein shield and polyvinyl alcohol is 40: 60; Boron solution is added to the spinning solution to form a spinning dope; the spinning dope is at a temperature of 80 ° (:, under normal pressure) The foaming was carried out for 5 hours, and the spinning process was carried out to prepare a protein synthetic fiber by a wet spinning process.
实施例 7: 将动物毛去脂去杂后浸泡在 PH为 1的水溶液中, 并进行搅拌, 在温度 80°C经过 3小时后分离提纯除去废渣, 用减调浸出液的等电点, 得分 离蛋白质; 将分离蛋白质溶于含有三乙醇胺的软水溶液中, 溶解温度为 85 °C , 溶解时间为 1. 8 小时, 制成蛋白质溶液; 将一定量水洗纯净的聚乙烯醇直接 加入蛋白质溶液中, 使它们共混共聚, 其温度緩慢升至 98°C , 保持 2. 8小时, 其间加入软水调节浓度, 制得含蛋白质和聚乙烯醇的浓度为 15%的纺丝溶液, 其中蛋白质和聚乙烯醇的干固量重量比为 75: 25 ; '向纺丝溶液中加入硼砂调 整粘度, 制成纺丝原液; 纺丝原液在温度 65 °C、 常压下静置脱泡 6小时, 进 入纺丝程序, 用湿法纺丝工艺制成蛋白质合成纤维。 Example 7: The animal hair was degreased and then immersed in an aqueous solution of pH 1 and stirred. After 3 hours at a temperature of 80 ° C, the separation and purification were carried out to remove the waste residue, and the isoelectric point of the leaching solution was used to separate. The protein is dissolved in a soft aqueous solution containing triethanolamine, the dissolution temperature is 85 ° C, the dissolution time is 1.8 hours, and the protein solution is prepared; a certain amount of washed pure polyvinyl alcohol is directly added to the protein solution, They were blended and copolymerized, and the temperature was slowly raised to 98 ° C for 2.8 hours, during which soft water was added to adjust the concentration to obtain a spinning solution containing protein and polyvinyl alcohol at a concentration of 15%, wherein protein and polyethylene. The dry weight ratio of alcohol is 75: 25; 'The borax is added to the spinning solution to adjust the viscosity to make the spinning dope; the spinning dope is allowed to defoam at a temperature of 65 °C for 6 hours under normal pressure. Silk process, a protein synthetic fiber is produced by a wet spinning process.
实施例 8: 将动物毛去脂去杂后浸泡在 PH为 0. 5的水溶液中, 并进行搅 拌, 在温度 60°C经过 2小时后分离提纯除去废渣, 用碱调浸出液的等电点, 得分离蛋白质; 将分离蛋白质溶于含有三乙醇胺的软水溶液中, 溶解温度为 40°C , 溶解时间为 3 小时, 制成蛋白质溶液; 将一定量水洗纯净的聚乙烯醇 直接加入蛋白质溶液中, 使它们共混共聚, 其温度緩慢升至 98 °C , 保持 3小
时, 其间加入软水调节浓度, 制得含蛋白质和聚乙烯醇的浓度为 11%的紡丝溶 液, 其中蛋白质和聚乙烯醇的干固量重量比为 90 : 10; 向纺丝溶液中加入硼 砂调整粘度, 制成纺丝原液; 纺丝原液在温度 75 °C、 常压下静置脱泡 5小 时, 进入纺丝程序, 用湿法纺丝工艺制成蛋白质合成纤维。 Example 8: The animal hair was degreased and then immersed in an aqueous solution having a pH of 0.5, and stirred. After 2 hours at a temperature of 60 ° C, the separation and purification were carried out to remove the waste residue, and the isoelectric point of the leachate was adjusted with a base. The protein is separated; the isolated protein is dissolved in a soft aqueous solution containing triethanolamine, the dissolution temperature is 40 ° C, and the dissolution time is 3 hours to prepare a protein solution; a certain amount of washed pure polyvinyl alcohol is directly added to the protein solution, They are blended and copolymerized, and the temperature is slowly raised to 98 °C, keeping 3 small At the same time, adding soft water to adjust the concentration to obtain a spinning solution containing protein and polyvinyl alcohol at a concentration of 11%, wherein the dry weight ratio of protein to polyvinyl alcohol is 90: 10; adding borax to the spinning solution The viscosity is adjusted to prepare a spinning dope; the spinning dope is allowed to defoam for 5 hours at a temperature of 75 ° C under normal pressure, and is subjected to a spinning process to form a protein synthetic fiber by a wet spinning process.
实施例 9: 将动物毛去脂去杂后浸泡在 PH为 0. 7的水溶液中, 并进行搅 拌,在温度 25Ό经过 7. 5小时后分离提纯除'去废渣, 用碱调浸出液的等电点, 得分离蛋白质; 将分离蛋白质溶于含有十二 基磺酸钠的软水溶液中, 溶解 温度为 20°C , 溶解时间为 3. 5小时, 制成蛋白质溶液; 将一定量水洗纯净的 聚乙烯醇直接加入蛋白质溶液中, 使它们共混共聚, 其温度緩慢升至 98°C , 保持 4小时, 其间加入软水调节浓度, 制得含蛋白质和聚乙烯醇的浓度为 15% 的纺丝溶液, 其中蛋白质和聚乙烯醇的干固量重量比为 15: 85; 向纺丝溶液 中加入硼酸调整粘度, 制成纺丝原液; 纺丝原液在温度 30°C、 真空条件下静 置脱泡 7. 5小时, 进入纺丝程序, 用干喷湿纺工艺制成蛋白质合成纤维。 Example 9: The animal hair was degreased and then immersed in an aqueous solution having a pH of 0.7, and stirred, and after 25 hours at a temperature of 25 Torr, the separation and purification were carried out except that the waste was removed, and the leaching solution was adjusted with alkali. The separation protein is dissolved in a soft aqueous solution containing sodium dodecyl sulfonate, the dissolution temperature is 20 ° C, the dissolution time is 3.5 hours, and the protein solution is prepared; Vinyl alcohol was directly added to the protein solution, and they were blended and copolymerized. The temperature was slowly raised to 98 ° C for 4 hours, and soft water was added thereto to adjust the concentration to obtain a spinning solution containing protein and polyvinyl alcohol at a concentration of 15%. , wherein the dry weight ratio of protein to polyvinyl alcohol is 15: 85; boric acid is added to the spinning solution to adjust the viscosity to prepare a spinning dope; the spinning dope is allowed to defoam at a temperature of 30 ° C under vacuum. 7. 5 hours, into the spinning process, using a dry spray wet spinning process to make protein synthetic fibers.
实施例 10: 将动物毛去脂去杂后浸泡在 PH为 0. 9的水溶液中 , 并进行搅 拌, 在温度 95°C经过 1. 5小时后分离提纯除去废渣, 用碱调浸出液的等电点, 得分离蛋白质; 将分离蛋白质溶于含有十二烷基磺酸钠的软水溶液中, 溶解 温度为 35 °C , 溶解时间为 4小时, 制成蛋白质溶液; 将一定量水洗纯净的聚 乙烯醇直接加入蛋白质溶液中, 使它们共混共聚, 其温度緩慢升至 98°C , 保 持 2 小时, 其间加入软水调节浓度, 制得含蛋白质和聚乙烯醇的浓度为 16% 的紡丝溶液, 其中蛋白质和聚乙烯醇的干固量重量比为 70: 30; 向纺丝溶液 中加入硼酸调整粘度, 制成纺丝原液; 纺丝原液在温度 40°C、 真空条件下静 置脱泡 5小时, 进入纺丝程序, 用干喷湿纺工艺制成蛋白质合成纤维。 Example 10: The animal hair was degreased and then immersed in an aqueous solution having a pH of 0.9, and stirred. After the temperature was 95 ° C for 1.5 hours, the separation and purification were carried out to remove the waste residue, and the alkali was used to adjust the isoelectricity of the leachate. Point, the protein is separated; the isolated protein is dissolved in a soft aqueous solution containing sodium dodecyl sulfate, the dissolution temperature is 35 ° C, the dissolution time is 4 hours, and the protein solution is prepared; the pure polyethylene is washed with a certain amount of water. The alcohol was directly added to the protein solution, and they were blended and copolymerized. The temperature was slowly raised to 98 ° C for 2 hours, and soft water was added thereto to adjust the concentration to obtain a spinning solution containing protein and polyvinyl alcohol at a concentration of 16%. The dry weight ratio of protein to polyvinyl alcohol is 70: 30; boric acid is added to the spinning solution to adjust the viscosity to prepare a spinning dope; the spinning dope is allowed to defoam at a temperature of 40 ° C under vacuum conditions. After hours, enter the spinning process and make a protein synthetic fiber by dry-jet wet spinning.
实施例 11:将人发去脂去杂后浸泡在 PH为 2. 8的水溶液中,并进行搅拌, 在温度 98°C经过 2小时后分离提纯除去废渣, 用碱调浸出液的等电点, 得人 发分离蛋白质; 将分离蛋白质溶于含有十二烷基磺酸钠的软水溶液中, 溶解
温度为 70°C, 溶解时间为 3小时, 制成蛋白质溶液; 将一定量水洗纯净的聚 乙浠醇直接加入蛋白质溶液中, 使它们共混共聚, 其温度緩慢升至 98°C, 保 持 1.5小时, 其间加入软水调节浓度, 制得含蛋白^和聚乙烯醇的浓度为 21% 的纺丝溶液, 其中蛋白质和聚乙烯醇的干固量重量比为 30 : 70; 向纺丝溶液 中加入硼酸调整粘度, 制成紡丝原液; 纺丝原液在温度 35°C、 真空条件下静 置脱泡 6.5小时, 进入纺丝程序, 用干喷湿纺工艺制成蛋白质合成纤维。 Example 11: The human hair was degreased and then immersed in an aqueous solution having a pH of 2.8, and stirred. After 2 hours at a temperature of 98 ° C, the separation and purification were carried out to remove the waste residue, and the isoelectric point of the leaching solution was adjusted with a base. The human hair is isolated; the isolated protein is dissolved in a soft aqueous solution containing sodium dodecyl sulfate, dissolved The temperature was 70 ° C, the dissolution time was 3 hours, and the protein solution was prepared. A certain amount of washed pure polyethylene glycol was directly added to the protein solution, and they were blended and copolymerized, and the temperature was slowly raised to 98 ° C, and kept at 1.5. Hours, during which soft water was added to adjust the concentration to obtain a spinning solution containing 21% of protein and polyvinyl alcohol, wherein the dry weight ratio of protein to polyvinyl alcohol was 30: 70; added to the spinning solution Boric acid adjusts the viscosity to make a spinning dope; the spinning dope is degassed at a temperature of 35 ° C under vacuum for 6.5 hours, enters the spinning process, and is made into a protein synthetic fiber by a dry-jet wet spinning process.
实施例 12:将动物毛和人发去脂去杂后,一起浸泡在 PH为 3的水溶液中, 并进行搅拌, 在温度 75°C经过 3小时后分离提纯除去废渣, 用碱调浸出液的 等电点, 得分离蛋白盾; 将分离蛋白质溶于含有十二烷基磺酸钠的软水溶液 中, 溶解温度为 80 °C, 溶解时间为 1.5小时, 制成蛋白质溶液; 将一定量水 洗纯净的聚乙烯醇直接加入蛋白质溶液中, 使它们共混共聚, 其温度緩慢升 至 98°C, 保持 3小时, 其间加入软水调节浓度, 制得含蛋白质和聚乙烯醇的 浓度为 25%的纺丝溶液, 其中蛋白质和聚乙浠醇的干固量重量比为 12 : 88; 向纺丝溶液中加入硼酸调整粘度, 制成纺丝原液; 纺丝原液在温度 33°C、 真 空条件下静置脱泡 3.5 小时, 进入纺丝程序, 用干喷湿纺工艺制成蛋白质合 成纤维。 Example 12: After the animal hair and the human hair were degreased, they were immersed in an aqueous solution of pH 3 and stirred, and after 3 hours at a temperature of 75 ° C, the separation and purification were carried out to remove the waste residue, and the alkali leaching solution was adjusted. The electric point is obtained by separating the protein shield; the separated protein is dissolved in a soft aqueous solution containing sodium dodecylsulfonate, the dissolution temperature is 80 ° C, the dissolution time is 1.5 hours, and the protein solution is prepared; The polyvinyl alcohol was directly added to the protein solution, and they were blended and copolymerized. The temperature was slowly raised to 98 ° C for 3 hours, and soft water was added thereto to adjust the concentration to obtain a spinning concentration of 25% containing protein and polyvinyl alcohol. Solution, wherein the dry weight ratio of protein to polyethylene glycol is 12: 88; adding boric acid to the spinning solution to adjust the viscosity to prepare a spinning dope; the spinning dope is allowed to stand at a temperature of 33 ° C under vacuum After defoaming for 3.5 hours, the spinning process was carried out, and the protein synthetic fiber was prepared by a dry-jet wet spinning process.
实施例 13: 将动物毛去脂去杂后浸泡在 PH为 1.3的水溶液中, 并进行搅 拌, 在温度 85°C经过 2.5小时后分离提纯除去废渣, 用碱调浸出液的等电点, 得分离蛋白质; 将分离蛋白质溶于含有三乙醇胺的软水溶液中, 溶解温度为 55°C, 溶解时间为 2 小时, 制成蛋白质溶液; 将一定量水洗純净的聚乙烯醇 直接加入蛋白质溶液中, 使它们共混共聚, 其温度緩慢升至 98Ό, 保持 2.5 小时, 其间加入软水调节浓度, 制得含蛋白质和聚乙烯醇的浓度为 29%的纺丝 溶液, 其中蛋白质和聚乙烯醇的干固量重量比为 80 : 20; 向纺丝溶液中加入 硼砂调整粘度, 制成纺丝原液; 纺丝原液在温度 5G° ( 、 常压下静置脱泡 8小 时, 进入纺丝程序, 用干喷湿纺工艺制成蛋白质合成纤维。
实施例 14: 将动物毛去脂去杂后浸泡在 PH为 1. 8的水溶液中, 并进行搅 拌,在温度 55 °C经过 4. 5小时后分离提纯除去废渣, 用减调浸出液的等电点, 得分离蛋白质; 将分离蛋白质溶于含有三乙醇胺的软水溶液中, 溶解温度为 45 °C , 溶解时间为 3. 2 小时, 制成蛋白质溶液; 将一定量水洗纯净的聚乙烯 醇直接加入蛋白质溶液中,使它们共混共聚,其温度緩慢升至 98 °C,保持 1. 8 小时, 其间加入软水调节浓度, 制得含蛋白质和聚乙烯醇的浓度为 32%的纺丝 溶液, 其中蛋白质和聚乙烯醇的干固量重量比为 55: 45; 向纺丝溶液中加入 硼砂调整粘度, 制成纺丝原液; 纺丝原液在温度 80°C、 常压下静置脱泡 4. 5 小时, 进入纺丝程序, 用干喷湿纺工艺制成蛋白质合成纤维。 Example 13: The animal hair was degreased and then immersed in an aqueous solution of pH 1.3, and stirred. After 2.5 hours at a temperature of 85 ° C, the separation and purification were carried out to remove the waste residue, and the isoelectric point of the leachate was adjusted with a base to obtain a separation. Protein; the isolated protein is dissolved in a soft aqueous solution containing triethanolamine, the dissolution temperature is 55 ° C, the dissolution time is 2 hours, and the protein solution is prepared; a certain amount of washed pure polyvinyl alcohol is directly added to the protein solution, so that They were blended and copolymerized, and the temperature was slowly raised to 98 Torr for 2.5 hours, during which soft water was added to adjust the concentration to obtain a spinning solution containing protein and polyvinyl alcohol at a concentration of 29%, wherein the dry weight of protein and polyvinyl alcohol The weight ratio is 80: 20; borax is added to the spinning solution to adjust the viscosity to make a spinning dope; the spinning dope is allowed to defoam for 8 hours at a temperature of 5 G ° (at normal pressure, into the spinning process, with dry spray) The wet spinning process produces protein synthetic fibers. Example 14: The animal hair was degreased and then immersed in an aqueous solution having a pH of 1.8, and stirred, and after 5 hours at a temperature of 55 ° C, the separation and purification were carried out to remove the waste residue, and the isoelectricity of the reduced leaching solution was used. Point, the protein is separated; the isolated protein is dissolved in a soft aqueous solution containing triethanolamine, the dissolution temperature is 45 ° C, the dissolution time is 3.2 hours, and the protein solution is prepared; a certain amount of washed pure polyvinyl alcohol is directly added In the protein solution, they were blended and copolymerized, and the temperature was slowly raised to 98 ° C for 1.8 hours, during which soft water was added to adjust the concentration to obtain a spinning solution containing 32% of protein and polyvinyl alcohol. The dry weight ratio of protein to polyvinyl alcohol is 55: 45; borax is added to the spinning solution to adjust the viscosity to prepare a spinning dope; the spinning dope is allowed to defoam at a temperature of 80 ° C under normal pressure. After 5 hours, enter the spinning process and make a protein synthetic fiber by dry-jet wet spinning.
实施例 15 : 将动物毛去脂去杂后浸泡在 PH为 2. 1的水溶液中, 并进行搅 拌, 在温度 35 °C经过 6. 5小时后分离提纯除去废渣, 用碱调浸出液的等电点, 得分离蛋白质; 将分离蛋白质溶于含有三乙醇胺的软水溶液中, 溶解温度为 65 °C , 溶解时间为 2. 5 小时, 制成蛋白质溶液; 将一定量水洗纯净的聚乙烯 醇直接加入蛋白质溶液中, 使它们共混共聚, 其温度緩慢升至 98 °C , 保持 3 小时, 其间加入软水调节浓度, 制得含蛋白质和聚乙烯醇的浓度为 35%的纺丝 溶液, 其中蛋白质和聚乙烯醇的干固量重量比为 35: 65; 向纺丝溶液中加入 硼砂调整粘度, 制成纺丝原液; 纺丝原液在温度 65 °C、 常压下静置脱泡 5. 5 小时, 进入纺丝程序 , 用干喷湿纺工艺制成蛋白质合成纤维。 Example 15: The animal hair was degreased and then immersed in an aqueous solution having a pH of 2.1, and stirred, and after 6 hours at a temperature of 35 ° C, the separation and purification were carried out to remove the waste residue, and the alkali was used to adjust the isoelectricity of the leachate. Point, the protein is separated; the isolated protein is dissolved in a soft aqueous solution containing triethanolamine, the dissolution temperature is 65 ° C, the dissolution time is 2.5 hours, and the protein solution is prepared; a certain amount of washed pure polyvinyl alcohol is directly added In the protein solution, they were blended and copolymerized, and the temperature was slowly raised to 98 ° C for 3 hours, during which soft water was added to adjust the concentration to obtain a spinning solution containing protein and polyvinyl alcohol at a concentration of 35%, in which protein and The sufficiency of the sulphide is 5. 5 hours. The spinning solution is placed at a temperature of 65 ° C. , into the spinning process, using dry-jet wet spinning process to make protein synthetic fibers.
实施例 16 : 将动物毛去脂去杂后浸泡在 PH为 2. 5的水溶液中, 并进行搅 拌, 在温度 45 °C经过 5. 5小时后分离提纯除去废渣, 用碱调浸出液的等电点, 得分离蛋白质; 将分离蛋白盾溶于含有三乙醇胺的软水溶液中, 溶解温度为 15 °C , 溶解时间为 3 小时, 制成蛋白质溶液; 将一定量水.洗純净的聚乙烯醇 直接加入蛋白质溶液中, 使它们共混共聚, 其温度緩慢升至 98 °C , 保持 2. 8 小时, 其间加入软水调节浓度, 制得含蛋白质和聚乙烯醇的浓度为 38%的纺丝 溶液, 其中蛋白质和聚乙烯醇的干固量重量比为 7: 93; 向纺丝溶液中加入硼
砂调整粘度, 制成纺丝原液; 纺丝原液在温度 75°C、 常压下静置脱泡 3小时, 进入纺丝程序, 用湿法纺丝工艺制成蛋白质合成纤维。 Example: The animal hair was degreased and then immersed in an aqueous solution having a pH of 2.5, and stirred. After 5 hours at a temperature of 45 ° C, the separation and purification were carried out to remove the waste residue, and the alkali was used to adjust the isoelectricity of the leachate. Point, the protein is separated; the separated protein shield is dissolved in a soft aqueous solution containing triethanolamine, the dissolution temperature is 15 ° C, the dissolution time is 3 hours, and the protein solution is prepared; a certain amount of water is washed. The pure polyvinyl alcohol is washed. Directly added to the protein solution, they were blended and copolymerized, and the temperature was slowly raised to 98 ° C for 2.8 hours, during which soft water was added to adjust the concentration to obtain a spinning solution containing 38% of protein and polyvinyl alcohol. , wherein the dry weight ratio of protein to polyvinyl alcohol is 7:93; boron is added to the spinning solution The sand is adjusted to a viscosity to prepare a spinning dope; the spinning dope is allowed to defoam for 3 hours at a temperature of 75 ° C under normal pressure, and is subjected to a spinning process to form a protein synthetic fiber by a wet spinning process.
实施例 17: 将动物毛去脂去杂后浸泡在 PH为 1. 5的水溶液中, 并进行搅 拌, 在温度 70°C经过 6小时后分离提纯除去废渣, 用碱调浸出液的等电点, 得分离蛋白质; 将分离蛋白质溶于含有十二烷基横酸钠的软水溶液中, 溶解 温度为 15°C , 溶解时间为 4小时, 制成蛋白质溶液; 将一定量水洗纯净的聚 乙烯醇直接加入蛋白质溶液中, 使它们共混共聚, 其温度緩慢升至 98°C , 保 持 3. 5小时, 其间加入软水调节浓度, 制得含蛋白质和聚乙烯醇的浓度为 20% 的纺丝溶液, 其中蛋白质和聚乙烯醇的干固量重量比为 85: 15; 向纺丝溶液 中加入硼酸调整粘度, 制成纺丝原液; 纺丝原液在温度 40°C、 真空条件下静 置脱泡 7. 5小时, 进入纺丝程序, 用干法纺丝工艺制成蛋白质合成纤维。 Example 17: The animal hair was degreased and then immersed in an aqueous solution having a pH of 1.5, and stirred. After 6 hours at a temperature of 70 ° C, the separation and purification were carried out to remove the waste residue, and the isoelectric point of the leachate was adjusted with a base. The protein is separated; the isolated protein is dissolved in a soft aqueous solution containing sodium dodecyl sulphate, the dissolution temperature is 15 ° C, the dissolution time is 4 hours, and a protein solution is prepared; a certain amount of water is washed directly with the pure polyvinyl alcohol. Adding to the protein solution, blending and copolymerizing them, the temperature is slowly raised to 98 ° C, and kept for 3.5 hours, during which soft water is added to adjust the concentration to obtain a spinning solution containing protein and polyvinyl alcohol at a concentration of 20%. The dry weight ratio of protein to polyvinyl alcohol is 85: 15; boric acid is added to the spinning solution to adjust the viscosity to prepare a spinning dope; the spinning dope is allowed to defoam at a temperature of 40 ° C under vacuum conditions. 5 hours, into the spinning process, using the dry spinning process to make protein synthetic fibers.
实施例 18:将动物毛去脂去杂后浸泡在 PH为 2的水溶液中 ,并进行搅拌, 在温度 40°C经过 7小时后分离提纯除去废渣, 用碱调浸出液的等电点, 得分 离蛋白质; 将分离蛋白质溶于含有十二烷基磺酸钠的软水溶液中, 溶解温度 为 30°C, 溶解时间为 2小时, 制成蛋白质溶液; 将一定量水洗纯净的聚乙烯 醇直接加入蛋白质溶液中, 使它们共混共聚, 其温度緩慢升至 98 °C , 保持 4 小时, 其间加入软水调节浓度, 制得含蛋白质和聚乙烯醇的浓度为 38%的纺丝 溶液, 其中蛋白质和聚乙烯醇的干固量重量比为 5: 95; 向纺丝溶液中加入硼 酸调整粘度, 制成纺丝原液; 纺丝原液在温度 37°C、真空条件下静置脱泡 6. 5 小时, 进入纺丝程序, 用干法纺丝工艺制成蛋白质合成纤维。 Example 18: Degrease the animal hair, and then immersed in an aqueous solution of pH 2, and stirred. After 7 hours at a temperature of 40 ° C, the separation and purification were carried out to remove the waste residue, and the isoelectric point of the leachate was adjusted with a base to obtain a separation. Protein; the isolated protein is dissolved in a soft aqueous solution containing sodium dodecyl sulfate, the dissolution temperature is 30 ° C, the dissolution time is 2 hours, and the protein solution is prepared; a certain amount of washed pure polyvinyl alcohol is directly added to the protein In the solution, they were blended and copolymerized, and the temperature was slowly raised to 98 ° C for 4 hours, during which soft water was added to adjust the concentration to obtain a spinning solution containing 38% of protein and polyvinyl alcohol, in which protein and poly 5小时,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,, Into the spinning process, the protein synthesis fiber is made by a dry spinning process.
实施例 19:将人发去脂去杂后浸泡在 PH为 2. 3的水溶液中,并进行搅拌, 在温度 90°C经过 4小时后分离提纯除去废渣, 用碱调浸出液的等电点, 得人 发分离蛋白质; 将分离蛋白质溶于含有十二烷基磺酸钠的软水溶液中, 溶解 温度为 60°C , 溶解时间为 1. 5小时, 制成蛋白质溶液; 将一定量水洗纯净的 聚乙烯醇直接加入蛋白质溶液中, 使它们共混共聚, 其温度緩慢升至 98°C,
保持 3小时, 其间加入软水调节浓度, 制得含蛋白质和聚乙烯醇的浓度为 34% 的纺丝溶液, 其中蛋白质和聚乙烯醇的干固量重量比为 50 : 50; 向纺丝溶液 中加入硼酸调整粘度, 制成纺丝原液; 纺丝原液在温度 34 °C、 真空条件下静 置脱泡 4小时, 进入纺丝程序, 用干法纺丝工艺制成蛋白质合成紆维。 Example 19: The human hair was degreased and then immersed in an aqueous solution having a pH of 2.3, and stirred. After 4 hours at a temperature of 90 ° C, the separation and purification were carried out to remove the waste residue, and the isoelectric point of the leachate was adjusted with a base. The human protein is separated into a protein; the isolated protein is dissolved in a soft aqueous solution containing sodium dodecyl sulfate, the dissolution temperature is 60 ° C, the dissolution time is 1.5 hours, and the protein solution is prepared; Polyvinyl alcohol is directly added to the protein solution, and they are blended and copolymerized, and the temperature is slowly raised to 98 ° C. Hold for 3 hours, add soft water to adjust the concentration, to obtain a spinning solution containing protein and polyvinyl alcohol at a concentration of 34%, wherein the dry weight ratio of protein to polyvinyl alcohol is 50: 50; into the spinning solution The boric acid was added to adjust the viscosity to prepare a spinning dope; the spinning dope was allowed to defoam for 4 hours under the condition of a temperature of 34 ° C under vacuum, and the spinning process was carried out, and the protein synthesis was carried out by a dry spinning process.
实施例 20: 将动物毛和人发去脂去杂后 , 一起浸泡在 PH为 2. 6的水溶液 中, 并进行搅拌, 在温度 20Ό经过 8小时后分离提纯除去废渣, 用碱调浸出 液的等电点, 得分离蛋白质; 将分离蛋白质溶于含有十二烷基磺酸钠的软水 溶液中, 溶解温度为 50°C, 溶解时间为 3. 8小时, 制成蛋白质溶液; 将一定 量水洗纯净的聚乙烯醇直接加入蛋白质溶液中, 使它们共混共聚, 其温度緩 慢升至 98 °C , 保持 1. 5小时, 其间加入软水调节浓度, 制得含蛋白质和聚乙 烯醇的浓度为 31%的纺丝溶液, 其中蛋白质和聚乙烯醇的干固量重量比为 65: 35 ; 向纺丝溶液中加入硼酸调整粘度, 制成纺丝原液; 纺丝原液在温度 30°C、 真空条件下静置脱泡 5. 5 小时, 进入纺丝程序, 用干法纺丝工艺制成 蛋白盾合成纤维。 Example 20: After the animal hair and the human hair were degreased, they were immersed in an aqueous solution having a pH of 2.6 and stirred. After 8 hours at a temperature of 20 Torr, the separation and purification were carried out to remove the waste residue, and the leaching solution was adjusted with a base. The protein is separated into a protein; the dissolved protein is dissolved in a soft aqueous solution containing sodium dodecyl sulfate, the dissolution temperature is 50 ° C, the dissolution time is 3.8 hours, and the protein solution is prepared; The polyvinyl alcohol was directly added to the protein solution, and they were blended and copolymerized. The temperature was slowly raised to 98 ° C for 1.5 hours, and soft water was added thereto to adjust the concentration to obtain a protein-containing and polyvinyl alcohol concentration of 31%. The spinning solution, wherein the dry weight ratio of protein to polyvinyl alcohol is 65: 35; adding boric acid to the spinning solution to adjust the viscosity to prepare a spinning dope; spinning dope at a temperature of 30 ° C under vacuum After standing defoaming for 5. 5 hours, the spinning process was carried out, and the protein shield synthetic fiber was prepared by a dry spinning process.
实施例 21 :将动物毛去脂去杂后浸泡在 PH为 3的水溶液中 ,并进行搅拌, 在温度 98 °C经过 1小时后分离提纯除去废渣, 用威调浸出液的等电点, 得分 离蛋白质; 将分离蛋白质溶于含有三乙醇胺的软水溶液中, 溶解温度为 25 °C, 溶解时间为 3. 5 小时, 制成蛋白质溶液; 将一定量水洗纯净的聚乙烯醇直接 加入蛋白质溶液中, 使它们共混共聚, 其温度緩慢升至 98 °C , 保持 2小时, 其间加入软水调节浓度, 制得含蛋白质和聚乙烯醇的浓度为 36%的纺丝溶液, 其中蛋白质和聚乙烯醇的干固量重量比为 17 : 83; 向纺丝溶液中加入硼砂调 整粘度, 制成纺丝原液; 纺丝原液在温度 80°C、 常压下静置脱泡 5小时, 进 入纺丝程序, 用干法紡丝工艺制成蛋白质合成纤维。 Example 21: The animal hair was degreased and then immersed in an aqueous solution of pH 3, and stirred. After 1 hour at a temperature of 98 ° C, the separation and purification were carried out to remove the waste residue, and the isoelectric point of the immersion liquid was separated. The protein is dissolved in a soft aqueous solution containing triethanolamine, the dissolution temperature is 25 ° C, the dissolution time is 3.5 hours, and the protein solution is prepared; a certain amount of washed pure polyvinyl alcohol is directly added to the protein solution, They were blended and copolymerized, and the temperature was slowly raised to 98 ° C for 2 hours, during which soft water was added to adjust the concentration to obtain a spinning solution containing protein and polyvinyl alcohol at a concentration of 36%, wherein protein and polyvinyl alcohol were used. The dry weight ratio is 17: 83; borax is added to the spinning solution to adjust the viscosity to make a spinning dope; the spinning dope is allowed to defoam for 5 hours at a temperature of 80 ° C under normal pressure, and enters the spinning process. The protein synthetic fiber is made by a dry spinning process.
实施例 22: 将动物毛去脂去杂后浸泡在 PH为 1. 1的水溶液中, 并进行搅 拌, 在温度 30°C经过 5小时后分离提纯除去废淦, 用碱调浸出液的等电点,
得分离蛋白质; 将分离蛋白质溶于含有三乙醇胺的软水溶液中, 溶解温度为Example 22: The animal hair was degreased and then immersed in an aqueous solution having a pH of 1.1, and stirred. After 5 hours at a temperature of 30 ° C, the separation and purification were carried out to remove the waste sputum, and the isoelectric point of the leaching solution was adjusted with alkali. , The protein is separated; the isolated protein is dissolved in a soft aqueous solution containing triethanolamine, and the dissolution temperature is
75 °C , 溶解时间为 2. 5 小时, 制成蛋白质溶液; 将一定量水洗纯净的聚乙烯 醇直接加入蛋白质溶液中,使它们共混共聚,其温度緩慢升至 98 °C ,保持 3. 2 小时,其间加入软水调节浓度, 制得含蛋白质和聚乙烯醇的浓度为 23%的纺丝 溶液, 其中蛋白质和聚乙烯醇的干固量重量比为 43: 57; 向纺丝溶液中加入 硼砂调整粘度, 制成纺丝原液; 纺丝原液在温度 7 Q°C、 常压下静置脱泡 3小 时, 进入纺丝程序, 用干法纺丝工艺制成蛋白盾合成纤维。 75 ° C, dissolution time of 2.5 hours, made into a protein solution; a certain amount of washed pure polyvinyl alcohol was directly added to the protein solution, so that they were blended copolymerization, the temperature slowly rose to 98 ° C, maintaining 3. 2 hours, during which soft water was added to adjust the concentration to obtain a spinning solution containing 23% of protein and polyvinyl alcohol, wherein the dry weight ratio of protein to polyvinyl alcohol was 43: 57; added to the spinning solution Borax adjusts the viscosity to make a spinning dope; the spinning dope is allowed to defoam for 3 hours at a temperature of 7 Q ° C under normal pressure, and enters a spinning process to form a protein shield synthetic fiber by a dry spinning process.
实施例 23:将动物毛去脂去杂后浸泡在 PH为 1的水溶液中,并进行搅拌, 在温度 80°C经过 3小时后分离提纯除去废渣, 用碱调浸出液的等电点, 得分 离蛋白质; 将分离蛋白质溶于含有三乙醇胺的软水溶液中, 溶解温度为 85 °C, 溶解时间为 1, 8 小时, 制成蛋白质溶液; 将一定量水洗纯净的聚乙烯醇直接 加入蛋白^溶液中, 使它们共混共聚, 其温度緩慢升至 98 °C , 保持 2. 5小时, 其间加入软水调节浓度, 制得含蛋白质和聚乙烯醇的浓度为 26%的纺丝溶液, 其中蛋白质和聚乙烯醇的干固量重量比为 38 : 62; 向纺丝溶液中加入硼 、调 整粘度, 制成纺丝原液; 纺丝原液在温度 60°C、 常压下静置脱泡 8小时, 进 入纺丝程序, 用干法纺丝工艺制成蛋白质合成纤维。 Example 23: Degrease the animal hair, and then immersed in an aqueous solution of pH 1 and stirred. After 3 hours at a temperature of 80 ° C, the separation and purification were carried out to remove the waste residue, and the isoelectric point of the leachate was adjusted with a base to obtain a separation. Protein; the isolated protein is dissolved in a soft aqueous solution containing triethanolamine, the dissolution temperature is 85 ° C, the dissolution time is 1, 8 hours, and the protein solution is prepared; a certain amount of washed pure polyvinyl alcohol is directly added to the protein solution , they were blended and copolymerized, the temperature was slowly raised to 98 ° C, and maintained for 2.5 hours, during which soft water was added to adjust the concentration to obtain a spinning solution containing protein and polyvinyl alcohol at a concentration of 26%, in which protein and poly The dry weight ratio of vinyl alcohol is 38: 62; boron is added to the spinning solution to adjust the viscosity to prepare a spinning dope; the spinning dope is allowed to defoam for 8 hours at a temperature of 60 ° C under normal pressure. Spinning process, using a dry spinning process to make protein synthetic fibers.
实施例 24: 将动物毛去脂去杂后浸泡在 PH为 0. 5的水溶液中, 并进行搅 拌, 在温度 60°C经过 2小时后分离提纯除去废渣, 用碱调浸出液的等电点, 得分离蛋白盾; 将分离蛋白质溶于含有三乙醇胺的软水溶液中, 溶解温度为 40°C , 溶解时间为 3 小时, 制成蛋白质溶液; 将一定量水洗纯净的聚乙烯醇 直接加入蛋白质溶液中, 使它们共混共聚, 其温度緩慢升至 98 °C , 保持 3小 时, 其间加入软水调节浓度, 制得含蛋白质和聚乙烯醇的浓度为 34%的纺丝溶 液, 其中蛋白质和聚乙烯醇的干固量重量比为 28 : 72; 向纺丝溶液中加入硼 砂调整粘度, 制成纺丝原液; 纺丝原液在温度 50°C、 常压下静置脱泡 6小时, 进入纺丝程序, 用干法纺丝工艺制成蛋白质合成纤维。
本发明中所提及的纺丝程序中的纺丝工艺均为现有技术 , 其中可釆用本 发明人在中国专利第 99116636. 1或 03111814. 3或 03111737. 6号专利申请文 件中所披露的工艺流程及参数, 在此不再详细说明。
Example 24: The animal hair was degreased and then immersed in an aqueous solution having a pH of 0.5, and stirred. After 2 hours at a temperature of 60 ° C, the separation and purification were carried out to remove the waste residue, and the isoelectric point of the leaching solution was adjusted with a base. Separating the protein shield; dissolving the isolated protein in a soft aqueous solution containing triethanolamine, dissolving at a temperature of 40 ° C, and dissolving for 3 hours to form a protein solution; adding a certain amount of washed pure polyvinyl alcohol directly to the protein solution , they were blended and copolymerized, and the temperature was slowly raised to 98 ° C for 3 hours, during which soft water was added to adjust the concentration to obtain a spinning solution containing protein and polyvinyl alcohol at a concentration of 34%, wherein protein and polyvinyl alcohol The dry weight ratio is 28: 72; borax is added to the spinning solution to adjust the viscosity to make a spinning dope; the spinning dope is allowed to defoam at a temperature of 50 ° C under normal pressure for 6 hours, and enters the spinning process. , a protein spinning synthetic fiber is produced by a dry spinning process. The spinning process in the spinning process mentioned in the present invention is a prior art, and the inventors of the present invention are disclosed in the patent application file of the Chinese Patent No. 99116636.1 or 03111181.4 or 03111737. The process flow and parameters are not described in detail here.