CN112064130A - Regenerated pulp, regenerated pulp viscose fiber and preparation method thereof - Google Patents

Regenerated pulp, regenerated pulp viscose fiber and preparation method thereof Download PDF

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Publication number
CN112064130A
CN112064130A CN202010916322.6A CN202010916322A CN112064130A CN 112064130 A CN112064130 A CN 112064130A CN 202010916322 A CN202010916322 A CN 202010916322A CN 112064130 A CN112064130 A CN 112064130A
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China
Prior art keywords
viscose
alkali
regenerated pulp
content
temperature
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CN202010916322.6A
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Chinese (zh)
Inventor
路宽
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Saideli Jiangsu Fiber Co ltd
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Saideli Jiangsu Fiber Co ltd
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Priority to CN202010916322.6A priority Critical patent/CN112064130A/en
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F2/00Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
    • D01F2/06Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D1/00Treatment of filament-forming or like material
    • D01D1/02Preparation of spinning solutions
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/06Wet spinning methods

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Artificial Filaments (AREA)

Abstract

The invention provides regenerated pulp, regenerated pulp viscose and a preparation method thereof, and particularly relates to the field of viscose, wherein firstly, the regenerated pulp is sequentially dipped, squeezed, aged, yellowed, dissolved, matured and defoamed to obtain viscose; spinning and post-treating the viscose to obtain viscose fibers; the concentration of primary dipping alkali is 222 +/-2 g/L, and the temperature of the primary dipping alkali is 53 +/-0.5 ℃; the concentration of secondary impregnation alkali is 193 +/-2 g/L, and the temperature of the secondary impregnation alkali is 52 +/-0.5 ℃; wherein, the squeezing comprises primary squeezing and secondary squeezing, and the specific technological parameters are that the content of methyl cellulose formed by the alkali cellulose after the primary squeezing is 22 +/-2 percent, and the alkali content is 16.5 +/-0.5 percent; after secondary pressing, the content of methyl cellulose consisting of the alkali cellulose is 34 +/-0.5 percent, and the alkali content is 15.0 +/-0.5 percent; the viscosity of the viscose is 25-30s, and the viscose contains 9.05-9.25% of methyl fiber; alkali content is 4.65-4.85%, viscosity is 32-42S, and ripening degree is 13-17m calculated by 10% ammonium chloride. The invention can improve the quality stability and performance of the regenerated pulp viscose fiber, not only ensures the resource utilization of raw materials, but also is beneficial to environmental protection.

Description

Regenerated pulp, regenerated pulp viscose fiber and preparation method thereof
Technical Field
The invention belongs to the field of viscose fibers, and particularly relates to regenerated pulp, regenerated pulp viscose fibers and a preparation method thereof.
Background
The viscose fiber is a main variety of artificial fiber, the main raw material of the viscose fiber is chemical pulp, including cotton pulp and wood pulp, and the viscose fiber is prepared by separating natural cellulose through chemical reaction and regenerating the natural cellulose; the demand of viscose fiber is increased year by year, the total output of the viscose fiber is steadily increased, although the reserve amount of wood pulp cellulose is larger, with the gradual improvement of the responsibility requirement of enterprises and the supervision of environmental problems, according to the sustainable policy, the management of forest protection is urgently needed to be practiced by finding alternative raw materials. The regenerated pulp is used as an alternative raw material, so that the reduction of resources and the recycling of wastes can be realized, the update of social resource concept is promoted, the resource consciousness, the environmental consciousness and the regenerated pulp fiber cultivation market are advocated in the whole society, the environmental protection is promoted by actual actions, and the method has important significance for protecting the environment, saving the resources and reducing the pollution. However, in the actual production process, if the regenerated pulp is directly used, the impact is generated on the existing production equipment and process parameters, the cost of manpower and material resources is increased, and meanwhile, the quality of finished products is fluctuated, so that the influence is generated on downstream spinning enterprises.
Disclosure of Invention
The invention aims to provide regenerated pulp, regenerated pulp viscose fiber and a preparation method thereof, which can improve the quality stability and performance of the regenerated pulp viscose fiber, ensure the resource utilization of raw materials and are beneficial to environmental protection.
The invention provides the following technical scheme:
regenerated pulp, regenerated pulp viscose fiber and a preparation method thereof, which comprises the following steps:
firstly, sequentially dipping, squeezing, ageing, yellowing, dissolving, curing and defoaming regenerated pulp to obtain viscose; spinning and post-treating the viscose to obtain viscose fibers;
wherein, the impregnation comprises primary impregnation and secondary impregnation, and the specific technological parameters are as follows:
the concentration of primary dipping alkali is 222 +/-2 g/L, and the temperature of the primary dipping alkali is 53 +/-0.5 ℃;
the concentration of secondary impregnation alkali is 193 +/-2 g/L, and the temperature of the secondary impregnation alkali is 52 +/-0.5 ℃;
wherein, squeeze and include once squeezing and squeezing for the second time, the concrete technological parameter is as follows:
the content of methyl cellulose formed by the alkali cellulose after primary pressing is 22 +/-2%, and the alkali content is 16.5 +/-0.5%;
after secondary pressing, the content of methyl cellulose consisting of the alkali cellulose is 34 +/-0.5 percent, and the alkali content is 15.0 +/-0.5 percent;
the viscosity of the viscose is 25-30s, and the viscose contains 9.05-9.25% of methyl fiber; alkali content is 4.65-4.85%, viscosity is 32-42S, and ripening degree is 13-17m calculated by 10% ammonium chloride.
Preferably, the regenerated pulp comprises 94.1% of methyl cellulose, 9.69% of water, 0.08% of ash, 9.4mpa.s of viscosity, 93.4% of whiteness, 10ppm of iron, 3.82% of pentosan, 0.2% of resin and CS210ml of a reaction mixture having a reactivity of 11.6S
Preferably, the recycled pulp is one or more of recycled cotton textile recycled pulp or recycled regenerated cellulose fiber textile recycled pulp or other recycled cellulose material recycled pulp.
Preferably, the composition of the spinning acid bath is 116g/L of sulfuric acid 114-;
the temperature of the spinning secondary bath is 80 +/-2 ℃, the acid content is 40-50g/L, and the draft ratio is 100 +/-10%;
the post-treatment desulfurization temperature is 80 +/-2 ℃, and the concentration is 1.0-1.4 g/L; the bleaching concentration is 0.1-0.3 g/L; the oil bath temperature is 60 +/-5 ℃, and the concentration is 9 +/-1 g/L; when drying, a three-section drying process is adopted, the temperature of the front region is less than or equal to 140 ℃, the temperature of the middle region is less than or equal to 140 ℃, and the temperature of the rear region is more than or equal to 40 ℃.
Preferably, concentrated alkali and desalted water are used for one-time soaking alkali liquor preparation, and hydraulic alkali preparation is stopped.
Preferably, the amount of the etiolating CS2 added in the preparation of viscose is 820L/800 KG/P.
Preferably, the concentration of the yellowing dissolving alkali in the preparation of the viscose is 17-18 g/l.
Preferably, the dry breaking strength of the viscose is more than or equal to 2.50CN/dtex, the wet breaking strength is more than or equal to 1.20CN/dtex, the oil content is 0.30 +/-0.05%, the residual sulfur content is less than or equal to 12.0mg/100g, the whiteness is 85.0 +/-1.5%, and the defects are less than or equal to 1.5mg/100 g.
The invention has the beneficial effects that:
the invention can realize the innovative use of raw materials, can realize the reduction of resources and the recycling of wastes, promotes the update of social resource concept, advocates resource consciousness, environmental consciousness and the market of cultivating regenerated pulp fibers in the whole society, promotes the environmental protection by actual action, and has important significance for protecting the environment, saving resources and reducing pollution; the invention can ensure the quality of finished products, can produce superior products, and achieves the purposes of technical innovation, environmental protection and clean production, thereby realizing the protection of the environment.
Detailed Description
Firstly, sequentially dipping, squeezing, ageing, yellowing, dissolving, curing and defoaming regenerated pulp to obtain viscose; the regenerated pulp comprises 94.1% of methyl fiber, 9.69% of water, 0.08% of ash, 9.4mpa.s of viscosity, 93.4% of whiteness, 10ppm of iron, 3.82% of pentosan, 0.2% of resin and CS210ml of the reaction performance was 11.6S; the adding amount of the etiolation CS2 in the preparation of the viscose is 820L/800 KG/P;
wherein, the impregnation comprises primary impregnation and secondary impregnation, and the specific technological parameters are that concentrated alkali and demineralized water are used for the primary impregnation, and hydraulic alkali is stopped for the primary impregnation. The concentration of primary impregnation alkali is 220g/L, and the temperature of the primary impregnation alkali is 52.5 ℃; the concentration of secondary impregnation alkali is 191g/L, and the temperature of the secondary impregnation alkali is 51.5 ℃; the concentration of etiolation dissolved alkali in the preparation of the viscose is 17 g/l;
wherein, the squeezing comprises primary squeezing and secondary squeezing, and the specific technological parameters are that the content of methyl fiber formed by the alkali cellulose after the primary squeezing is 20 percent, and the alkali content is 16 percent; after secondary pressing, the content of methyl cellulose consisting of the alkali cellulose is 33.5 percent, and the alkali content is 14.5 percent;
the viscosity of the viscose is 25s, and the content of methyl cellulose is 9.05 percent; alkali content is 4.65%, viscosity is 32S, and the ripening degree is 13m in terms of 10% ammonium chloride;
then spinning and post-treating the viscose to obtain viscose fibers, wherein the dry breaking strength of the viscose fibers is 2.50CN/dtex, the wet breaking strength is 1.20CN/dtex, the oil content is 0.25 percent, the residual sulfur content is 12.0mg/100g, the whiteness is 83.5 percent, and the defects are 1.5mg/100 g; the composition of the spinning acid bath is 114g/L of sulfuric acid, 9.0g/L of zinc sulfate, 1.310 of specific gravity and 45.5 ℃ of acid temperature;
the temperature of the spinning secondary bath is 78 ℃, the acid content is 40g/L, and the drafting rate is 90 percent; the post-treatment desulfurization temperature is 78 ℃, and the concentration is 1.0 g/L; the bleaching concentration is 0.1 g/L; the oil bath temperature is 55 ℃, and the concentration is 8 g/L; when drying, a three-section drying process is adopted, wherein the temperature of the front region is 140 ℃, the temperature of the middle region is 140 ℃, and the temperature of the rear region is 40 ℃.
Example 2
Firstly, the regenerated pulp is sequentially dipped, squeezed, aged and yellowed,Dissolving, curing and defoaming to obtain viscose; the regenerated pulp comprises 94.1% of methyl fiber, 9.69% of water, 0.08% of ash, 9.4mpa.s of viscosity, 93.4% of whiteness, 10ppm of iron, 3.82% of pentosan, 0.2% of resin and CS210ml of the reaction performance was 11.6S; the adding amount of the etiolation CS2 in the preparation of the viscose is 820L/800 KG/P;
wherein, the impregnation comprises primary impregnation and secondary impregnation, and the specific technological parameters are that concentrated alkali and demineralized water are used for the primary impregnation, and hydraulic alkali is stopped for the primary impregnation. The concentration of primary impregnation alkali is 224g/L, and the temperature of the primary impregnation alkali is 53 ℃; the concentration of secondary impregnation alkali is 193g/L, and the temperature of the secondary impregnation alkali is 52 ℃; the concentration of etiolation dissolved alkali in the preparation of the viscose is 18 g/l;
wherein, the squeezing comprises primary squeezing and secondary squeezing, and the specific technological parameters are that the content of methyl fiber formed by the alkali cellulose after the primary squeezing is 24 percent, and the alkali content is 17 percent; after secondary pressing, the content of methyl fiber consisting of the alkali cellulose is 34 percent, and the alkali content is 15.0 percent;
the viscosity of the viscose is 30s, and the viscose contains 99.25 percent of methyl cellulose; alkali content of 44.85%, viscosity of 42S, and ripening degree of 17m in terms of 10% ammonium chloride;
then spinning and post-treating the viscose to obtain viscose fibers, wherein the dry breaking strength of the viscose fibers is 3CN/dtex, the wet breaking strength of the viscose fibers is 1.5CN/dtex, the oil content is 0.30 percent, the residual sulfur content is 11.0mg/100g, the whiteness is 85.0 percent, and the defects are 1.4mg/100 g; the composition of the spinning acid bath is 116g/L of sulfuric acid, 10.0g/L of zinc sulfate, 1.330 of specific gravity and 46.5 ℃ of acid temperature;
the temperature of the spinning secondary bath is 80 ℃, the acid content is 50g/L, and the drafting rate is 100 percent; the post-treatment desulfurization temperature is 80 ℃, and the concentration is 1.4 g/L; the bleaching concentration is 0.3 g/L; the oil bath temperature is 60 ℃, and the concentration is 9 g/L; when drying, a three-section drying process is adopted, wherein the temperature of the front region is 135 ℃, the temperature of the middle region is 135 ℃, and the temperature of the rear region is 45 ℃.
Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art will understand that various changes, modifications and substitutions can be made without departing from the spirit and scope of the invention as defined by the appended claims. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (8)

1. A method for preparing regenerated pulp and regenerated pulp viscose fiber is characterized in that: firstly, sequentially dipping, squeezing, ageing, yellowing, dissolving, curing and defoaming regenerated pulp to obtain viscose; spinning and post-treating the viscose to obtain viscose fibers;
wherein, the impregnation comprises primary impregnation and secondary impregnation, and the specific technological parameters are as follows:
the concentration of primary dipping alkali is 222 +/-2 g/L, and the temperature of the primary dipping alkali is 53 +/-0.5 ℃;
the concentration of secondary impregnation alkali is 193 +/-2 g/L, and the temperature of the secondary impregnation alkali is 52 +/-0.5 ℃;
wherein, squeeze and include once squeezing and squeezing for the second time, the concrete technological parameter is as follows:
the content of methyl cellulose formed by the alkali cellulose after primary pressing is 22 +/-2%, and the alkali content is 16.5 +/-0.5%;
after secondary pressing, the content of methyl cellulose consisting of the alkali cellulose is 34 +/-0.5 percent, and the alkali content is 15.0 +/-0.5 percent;
the viscosity of the viscose is 25-30s, and the viscose contains 9.05-9.25% of methyl fiber; alkali content is 4.65-4.85%, viscosity is 32-42S, and ripening degree is 13-17m calculated by 10% ammonium chloride.
2. Regenerated pulp and regenerated pulp viscose fiber are characterized in that: the regenerated pulp comprises 94.1% of methyl fiber, 9.69% of water, 0.08% of ash, 9.4mpa.s of viscosity, 93.4% of whiteness, 10ppm of iron, 3.82% of pentosan, 0.2% of resin and CS210ml had a reactivity of 11.6S.
3. A process for preparing regenerated pulp and regenerated pulp viscose fibres according to claim 1, characterised in that: the regenerated pulp is one or more of regenerated pulp of recycled cotton textiles or regenerated pulp of recycled cellulose fibers textiles or regenerated pulp of other recycled cellulose materials.
4. A process for preparing regenerated pulp and regenerated pulp viscose fibres according to claim 1, characterised in that: the composition of the spinning acid bath is 116g/L of sulfuric acid 114-;
the temperature of the spinning secondary bath is 80 +/-2 ℃, the acid content is 40-50g/L, and the draft ratio is 100 +/-10%;
the post-treatment desulfurization temperature is 80 +/-2 ℃, and the concentration is 1.0-1.4 g/L; the bleaching concentration is 0.1-0.3 g/L; the oil bath temperature is 60 +/-5 ℃, and the concentration is 9 +/-1 g/L; when drying, a three-section drying process is adopted, the temperature of the front region is less than or equal to 140 ℃, the temperature of the middle region is less than or equal to 140 ℃, and the temperature of the rear region is more than or equal to 40 ℃.
5. A process for preparing regenerated pulp and regenerated pulp viscose fibres according to claim 1, characterised in that: the first dipping alkali liquor is prepared by using concentrated alkali and desalted water, and the hydraulic alkali is stopped.
6. A process for preparing regenerated pulp and regenerated pulp viscose fibres according to claim 1, characterised in that: the addition amount of the etiolation CS2 in the preparation of the viscose is 820L/800 KG/P.
7. A process for preparing regenerated pulp and regenerated pulp viscose fibres according to claim 1, characterised in that: the concentration of the etiolation dissolved alkali in the preparation of the viscose is 17-18 g/l.
8. A process for preparing regenerated pulp and regenerated pulp viscose fibres according to claim 1, characterised in that: the dry breaking strength of the viscose fiber is more than or equal to 2.50CN/dtex, the wet breaking strength is more than or equal to 1.20CN/dtex, the oil content is 0.30 +/-0.05 percent, the residual sulfur content is less than or equal to 12.0mg/100g, the whiteness is 85.0 +/-1.5 percent, and the defects are less than or equal to 1.5mg/100 g.
CN202010916322.6A 2020-09-03 2020-09-03 Regenerated pulp, regenerated pulp viscose fiber and preparation method thereof Pending CN112064130A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101372766A (en) * 2008-10-05 2009-02-25 山东海龙股份有限公司 Technological process for producing viscose fiber filament by secondary impregnation production
CN103556281A (en) * 2013-11-07 2014-02-05 唐山三友集团兴达化纤有限公司 Method for producing high-wet-modulus regenerated cellulose fibers from bamboo pulp
CN106757461A (en) * 2016-12-15 2017-05-31 山东银鹰化纤有限公司 A kind of half wet pulp prepares the preparation method of alkali cellulose and rayon spinning glue
TW201938590A (en) * 2018-01-15 2019-10-01 奧地利商蘭仁股份有限公司 Shaped body of cellulose incorporated in spandex and manufacturing process
US20200095395A1 (en) * 2018-01-12 2020-03-26 Tyton Biosciences, Llc Methods for recycling cotton and polyester fibers from waste textiles
CN111304767A (en) * 2020-02-17 2020-06-19 河北吉藁化纤有限责任公司 Preparation method for producing regenerated cellulose fiber by using waste textile regenerated pulp and regenerated cellulose fiber
US20200232162A1 (en) * 2017-04-27 2020-07-23 Infinited Fiber Company Oy Treatment process for textile-based materials

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101372766A (en) * 2008-10-05 2009-02-25 山东海龙股份有限公司 Technological process for producing viscose fiber filament by secondary impregnation production
CN103556281A (en) * 2013-11-07 2014-02-05 唐山三友集团兴达化纤有限公司 Method for producing high-wet-modulus regenerated cellulose fibers from bamboo pulp
CN106757461A (en) * 2016-12-15 2017-05-31 山东银鹰化纤有限公司 A kind of half wet pulp prepares the preparation method of alkali cellulose and rayon spinning glue
US20200232162A1 (en) * 2017-04-27 2020-07-23 Infinited Fiber Company Oy Treatment process for textile-based materials
US20200095395A1 (en) * 2018-01-12 2020-03-26 Tyton Biosciences, Llc Methods for recycling cotton and polyester fibers from waste textiles
TW201938590A (en) * 2018-01-15 2019-10-01 奧地利商蘭仁股份有限公司 Shaped body of cellulose incorporated in spandex and manufacturing process
CN111304767A (en) * 2020-02-17 2020-06-19 河北吉藁化纤有限责任公司 Preparation method for producing regenerated cellulose fiber by using waste textile regenerated pulp and regenerated cellulose fiber

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