CN115707805A - Method for producing lyocell fibers by using sulfite cooking chemical papermaking pulp - Google Patents

Method for producing lyocell fibers by using sulfite cooking chemical papermaking pulp Download PDF

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CN115707805A
CN115707805A CN202110946788.5A CN202110946788A CN115707805A CN 115707805 A CN115707805 A CN 115707805A CN 202110946788 A CN202110946788 A CN 202110946788A CN 115707805 A CN115707805 A CN 115707805A
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pulp
sulfite
cooking
acid
lyocell
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李孝亭
葛文越
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Shanghai Kaixin Isolation Technology Co ltd
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Shanghai Kaixin Isolation Technology Co ltd
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Abstract

The invention relates to the technical field of lyocell fiber production, in particular to a method for producing lyocell fiber by using sulfite cooking chemical paper making pulp. In the invention, a sulfite cooking modification process is embedded in the existing production process of the lyocell fiber, and the lyocell fiber is produced by using chemical pulp, thereby reducing the environmental pollution and solving the problems of raw material shortage and high preparation cost of the lyocell fiber; the fibers are degraded by acid hydrolysis, the polymerization degree required by the lyocell fibers is achieved, and the acid hydrolysis liquid can be recycled, so that the method is economical and environment-friendly; sulfite is used to prevent the accumulation of acid soluble lignin.

Description

Method for producing lyocell fibers by using sulfite cooking chemical papermaking pulp
Technical Field
The invention relates to the technical field of lyocell fiber production, in particular to a method for producing lyocell fiber by using sulfite cooking chemical papermaking pulp.
Background
The lyocell fiber takes natural plant fiber as a raw material, has various excellent properties of natural fiber and synthetic fiber, and is known as a product with the most value in the history of artificial fiber for nearly half century. The raw materials are natural cellulose in nature, the production process has no chemical reaction, the used solvent is nontoxic, the recovery rate of the solvent is up to 99.7 percent, and the fiber is energy-saving, environment-friendly and can be continuously developed and praised as green fiber.
However, the wood resource for producing the lyocell fiber is relatively scarce in China, and a large amount of wood and lyocell fiber pulp are imported each year for producing the lyocell fiber, so that a large amount of financial resources are consumed.
Disclosure of Invention
Aiming at the problems of shortage of raw materials and high preparation cost of the lyocell fibers, the invention aims to provide a method for producing the lyocell fibers by using sulfite cooking chemical paper pulp, namely, a sulfite cooking modification process is embedded in the existing production process of the lyocell fibers, and the lyocell fibers are produced by using chemical pulp.
The purpose of the invention can be realized by the following technical scheme:
the invention provides a method for producing lyocell fibers by using sulfite cooking chemical pulping, which comprises the following steps:
(1) Crushing the chemical paper making pulp, adding acid and sulfite for cooking, degrading fiber to reach the polymerization degree required by the lyocell pulp, and reducing the ash content of the paper pulp;
(2) Washing the cooked paper pulp by a pulp washer, and concentrating the paper pulp to the required concentration by a thickener;
(3) The concentrated paper pulp is mixed with Lyocell-grade dissolving pulp in any proportion independently or enters the existing Lyocell fiber production process.
In one embodiment of the present invention, in step (1), the chemical paper pulp is a softwood or hardwood chemical paper pulp with >81% cellulose, >85% whiteness, and >700 degree of polymerization.
In one embodiment of the present invention, in step (1), the packaging form of the chemical pulp includes, but is not limited to, roll, sheet, block.
In one embodiment of the present invention, in step (1), the crushing of the chemical pulp includes, but is not limited to, hydraulic pulping, dry pulping.
In one embodiment of the present invention, in the step (1), the acid includes an organic acid and an inorganic acid; the organic acids include, but are not limited to, acetic acid, citric acid, lactic acid; the inorganic acid includes, but is not limited to, sulfuric acid, phosphoric acid, hydrochloric acid.
In one embodiment of the present invention, in step (1), the acid pH is preferably 2 to 4.
In one embodiment of the present invention, in step (1), the sulfite includes, but is not limited to, sodium bisulfite, magnesium sulfite.
In one embodiment of the present invention, in the step (1), the sulfite concentration is preferably 0.1 to 2% by mass.
In one embodiment of the present invention, in the step (1), the solid-to-liquid ratio is 1:5 to 1:9, the mass concentration of the sulfite is 0.1 to 2 percent, and the pH is controlled to be 2 to 4.
In one embodiment of the present invention, in the step (1), the cooking process includes batch cooking, continuous cooking.
In one embodiment of the invention, in the step (1), the cooking temperature in the cooking process is 120-170 ℃, and the temperature is kept for 30-120min.
In one embodiment of the present invention, in step (1), the cooking liquor obtained after the cooking of the pulp is completed may be directly reused, or may be passed through a membrane separation system, and the low molecular weight monosaccharides and oligosaccharides permeate through the membrane to form a filtrate, and the organic matter with a larger molecular weight is retained by the membrane surface to form a concentrated solution for the production of dye dispersants, rubber aids, water reducers, etc.
In one embodiment of the invention, the filtrate can be used for the production of xylo-oligosaccharides, xylose, mannose, arabinose.
In one embodiment of the invention, in the step (3), the water content of the concentrated pulp is 1-99%, including a liquid state and a drying state; preferably in liquid form, so that the process can be directly embedded into the existing lyocell fibre production process, reducing cost.
In one embodiment of the present invention, in step (3), the concentrated pulp may be directly used in the lyocell production process, or may be mixed with lyocell-grade dissolving pulp in any proportion, and the mixture is fed into the lyocell production process, which is an existing general process.
The pulp for the lyocell has larger price difference with bulk chemical paper-making pulp due to the characteristics, and the pulp for the lyocell can reduce the import of the pulp for the lyocell, reduce the environmental pollution and reduce the production cost for manufacturing the lyocell by adding the pulp for the lyocell and the special pulp for the lyocell in any proportion after the chemical paper-making pulp is steamed and modified by sulfite; therefore, the use of chemical pulp for the production of lyocell fibers is the goal of the lyocell industry in our country.
Compared with the prior art, the invention has the following advantages:
(1) The chemical pulp is used for manufacturing the lyocell fiber, so that the complex manufacturing process of the lyocell pulp is saved, the environmental pollution is reduced, and the production cost of the lyocell fiber is reduced.
(2) The core of the invention is acid hydrolysis of the fiber to achieve the degree of polymerization required by the lyocell fiber, wherein the acid hydrolysis liquid can be recycled, and the method is economical and environment-friendly.
(3) In the delignification process of the pulp treatment, the sulfite also plays a role in preventing the accumulation of acid-soluble lignin, and the byproduct sodium lignosulfonate can also be recycled as a product.
Detailed Description
The purpose of the invention can be realized by the following technical scheme:
the invention provides a method for producing lyocell fibers by using sulfite cooking chemical pulping, which comprises the following steps:
(1) Crushing the chemical paper making pulp, adding acid and sulfite for cooking, degrading fiber to reach the polymerization degree required by the lyocell pulp, and reducing the ash content of the paper pulp;
(2) Washing the cooked paper pulp by a pulp washer, and concentrating the paper pulp to the required concentration by a thickener;
(3) The concentrated paper pulp is mixed with Lyocell-grade dissolving pulp in any proportion independently or enters the existing Lyocell fiber production process.
In one embodiment of the present invention, in step (1), the chemical paper pulp is a softwood or hardwood chemical paper pulp with >81% cellulose, >85% whiteness, and >700 degree of polymerization.
In one embodiment of the present invention, in step (1), the packaging form of the chemical pulp includes, but is not limited to, roll, sheet, block.
In one embodiment of the present invention, in step (1), the crushing of the chemical pulp includes, but is not limited to, hydraulic pulp crushing and dry pulp crushing.
In one embodiment of the present invention, in the step (1), the acid includes an organic acid and an inorganic acid; the organic acids include, but are not limited to, acetic acid, citric acid, lactic acid; the inorganic acid includes, but is not limited to, sulfuric acid, phosphoric acid, hydrochloric acid.
In one embodiment of the present invention, in step (1), the acid pH is preferably 2 to 4.
In one embodiment of the present invention, in step (1), the sulfite includes, but is not limited to, sodium bisulfite, magnesium sulfite.
In one embodiment of the present invention, in the step (1), the sulfite concentration is preferably 0.1 to 2% by mass.
In one embodiment of the present invention, in the step (1), the solid-to-liquid ratio is 1:5 to 1:9, the mass concentration of the sulfite is 0.1 to 2 percent, and the pH is controlled to be 2 to 4.
In one embodiment of the present invention, in the step (1), the cooking process includes batch cooking, continuous cooking.
In one embodiment of the invention, in the step (1), the cooking temperature in the cooking process is 120-170 ℃, and the temperature is kept for 30-120min.
In one embodiment of the present invention, in step (1), the cooking liquor obtained after the cooking of the pulp is completed may be directly reused, or may be passed through a membrane separation system, and the low molecular weight monosaccharides and oligosaccharides permeate through the membrane to form a filtrate, and the organic matter with a larger molecular weight is retained by the membrane surface to form a concentrated solution for the production of dye dispersants, rubber aids, water reducers, etc.
In one embodiment of the invention, the filtrate can be used for the production of xylo-oligosaccharides, xylose, mannose, arabinose.
In one embodiment of the invention, in the step (3), the water content of the concentrated pulp is 1-99%, including a liquid state and a drying state; preferably in liquid form, so that the process can be directly embedded into the existing lyocell fibre production process, reducing cost.
In one embodiment of the present invention, in step (3), the concentrated pulp may be directly used in the lyocell production process, or may be mixed with lyocell-grade dissolving pulp in any proportion, and the mixture is fed into the lyocell production process, which is an existing general process.
The present invention will be described in detail with reference to specific examples.
Example 1
This example provides a method of producing lyocell fibers using sulfite cooking chemical pulping, comprising the steps of:
(1) The chemical pulp sheet was cut into 5 by 5 cm pieces.
(2) 12 liters of water are first heated to 40 ℃ in a cooking pot, and then 100 g of sulfite, 300 ml of acid and 2 kg of chemical paper pulp board in dry weight are added in sequence.
(3) Screwing down the pot cover, controlling the heating speed, short-time deflating at 100 ℃, releasing pressure when the temperature is raised to 150 ℃ on the basis of no temperature drop, and then preserving the heat for 30 minutes.
(4) After the temperature is kept for 30 minutes, the pressure is released to the normal pressure, the pot cover is opened, and the slurry is put into a 60-mesh net bag.
(5) And (3) tightening the mesh bag, putting the mesh bag into a spin dryer for spin-drying, washing the mesh bag to be neutral by using clean water, and then spin-drying the mesh bag to reach the concentration of 33 percent, wherein the whiteness of the obtained paper pulp is more than 85 degrees.
(6) The pulp samples were weighed and tested according to the current lyocell enterprise assay method, with the results shown in table 1.
(7) And (5) dissolving the paper pulp obtained in the step (5) by 4-methylmorpholine-N-oxide (NMMO) and then entering a Lyocell production process.
TABLE 1 indexes of modified pulp obtained in example 1
Index (I) The modified pulp of the process Pulp for lyocell fibers
Degree of polymerization 502 480-550
Viscosity (cp) 11.46 10-12
All-grass of Chinese starjasmine 88% 88%-94%
Ash content% 0.07 ≤0.1%
Reactivity performance 3”54
Lignin content% 0.1 ≤0.1%
Example 2
The present embodiment provides a method for producing lyocell fibers using sulfite-cooked chemical pulping, comprising the steps of:
(1) The chemical pulp sheet was cut into 5 by 5 cm pieces.
(2) Firstly, 15 liters of water is heated to 60 ℃ in a cooking pot, and then 100 g of sulfite, 200 ml of acid and 2 kg of chemical paper-making pulp board with dry weight are added in sequence.
(3) Screwing down the pot cover, controlling the temperature rise speed, deflating for 1 minute at 115 ℃, releasing pressure for 1-2 minutes when the temperature rises to 145 ℃, and keeping the temperature for 60 minutes after the temperature does not drop.
(4) After keeping the temperature for 60 minutes, the pressure is released to the normal pressure, the pot cover is opened, and the faint yellow slurry is put into a 60-mesh net bag.
(5) And (3) tightening the mesh bag, putting the mesh bag into a spin dryer for spin-drying, washing the mesh bag to be neutral by using clean water, and then spin-drying the mesh bag to 33% of concentration, wherein the whiteness of the paper pulp is more than 85 degrees.
(6) The pulp samples were weighed and tested according to the current lyocell enterprise assay method, with the results shown in table 2.
(7) And (5) dissolving the paper pulp obtained in the step (5) by NMMO and then entering a lyocell production process.
TABLE 2 indexes of modified slurry obtained in example 2
Index (I) The modified pulp of the process Pulp for lyocell fibers
Degree of polymerization 496 480-550
Viscosity (cp) 10.48 10-12
All-grass of Chinese starjasmine 89% 88%-94%
Ash content% 0.08% ≤0.1%
Reactivity performance 2”94
The content of lignin% 0.99 ≤0.1%
Example 3
This example provides a method of producing lyocell fibers using sulfite cooking chemical pulping, comprising the steps of:
(1) The chemical pulp sheet was cut into 5 by 5 cm pieces.
(2) Firstly, heating 10L of the recovered liquid to 50 ℃ in a cooking pot, and then sequentially adding 60 g of sulfite, 180 ml of acid and 1.5 kg of chemical papermaking pulp board in dry weight.
(3) Screwing down the pot cover, controlling the heating speed, deflating at 115 ℃, releasing pressure for 1-2 minutes when the temperature is raised to 145 ℃, keeping the temperature for 50 minutes after the temperature is not reduced.
(4) After the temperature is kept for 50 minutes, the pressure is released to the normal pressure, the pot cover is opened, and the faint yellow slurry is put into a 60-mesh net bag.
(5) And (3) tightening the mesh bag, putting the mesh bag into a spin dryer for spin-drying, washing the mesh bag to be neutral by using clean water, and then spin-drying the mesh bag to 33% of concentration, wherein the whiteness of the paper pulp is more than 85 degrees.
(6) Pulp samples were weighed and tested according to the current lyocell enterprise assay with results as shown in table 3.
(7) And (5) dissolving the paper pulp obtained in the step (5) by NMMO and then entering a lyocell production process.
TABLE 3 indexes of modified slurry obtained in example 3
Figure BDA0003216926760000061
Figure BDA0003216926760000071
The embodiments described above are described to facilitate an understanding and appreciation of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make modifications and alterations without departing from the scope of the present invention.

Claims (10)

1. A method of producing lyocell fibre using sulfite cooking chemical pulping, comprising the steps of:
(1) Crushing chemical paper making pulp, adding acid and sulfite for cooking, degrading fiber to reach the required polymerization degree of 480-550 of the lyocell pulp, and reducing the ash content of the pulp to be lower than 0.1%;
(2) Washing the steamed paper pulp by a pulp washer, and concentrating by a thickener;
(3) And (3) mixing the concentrated paper pulp alone or with the lyocell-grade dissolving pulp in proportion, and entering the existing lyocell fiber production process.
2. The method for producing lyocell fiber using sulfite cooking chemical pulp, according to claim 1, wherein in the step (1), the chemical paper pulp is softwood or hardwood chemical pulp with cellulose >81%, whiteness >85%, and degree of polymerization > 700.
3. The method for producing lyocell fibers using sulfite cooking chemical pulp, according to claim 1, wherein in step (1), the crushing of said chemical pulp includes but is not limited to hydraulic pulping, dry pulping.
4. The method for producing lyocell fiber using sulfite cooking chemical pulping according to claim 1, wherein in the step (1), the acid includes an organic acid, an inorganic acid; the organic acids include, but are not limited to, acetic acid, citric acid, lactic acid; the inorganic acids include, but are not limited to, sulfuric acid, phosphoric acid, hydrochloric acid;
the pH of the acid is 2-4.
5. The method for producing lyocell fiber using sulfite cooking chemical pulping according to claim 1, wherein in step (1), the sulfite includes but is not limited to sodium bisulfite, magnesium sulfite;
the mass concentration of the sulfite is 0.1-2%.
6. The method for producing lyocell fibers using sulfite cooking chemical pulping according to claim 1, wherein in the step (1), the solid-to-liquid ratio is 1:5 to 1:9, the mass concentration of the sulfite is 0.1 to 2 percent, and the pH is controlled to be 2 to 4.
7. A method for producing lyocell fibre from sulfite cooking chemi-pulp in accordance with claim 1, wherein in step (1), the cooking process comprises batch cooking and continuous cooking.
8. The method for producing lyocell fiber using sulfite cooking chemical pulp according to claim 1, wherein the cooking temperature in the step (1) is 120 to 170 ℃ and the temperature is maintained for 30 to 120min.
9. The method for producing lyocell fibers from sulfite cooking chemical pulp according to claim 1, wherein in step (1), the cooking liquor obtained after completion of the cooking of the pulp includes, but is not limited to, direct reuse, treatment with a membrane separation system;
the cooking liquor passes through a membrane separation system to form filtrate through the medium and small molecular weight monosaccharides and oligosaccharides during treatment, and organic matters with larger molecular weight are intercepted by the surface of a membrane to form concentrated liquor.
10. The method for producing lyocell fiber using sulfite cooking chemical pulp according to claim 1, wherein the water content of the concentrated pulp in the step (3) is 1 to 99%.
CN202110946788.5A 2021-08-18 2021-08-18 Method for producing lyocell fibers by using sulfite cooking chemical papermaking pulp Pending CN115707805A (en)

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JP2009213389A (en) * 2008-03-10 2009-09-24 Nippon Paper Chemicals Co Ltd System for producing bioethanol using lignocellulose as raw material
US20090312536A1 (en) * 2006-05-10 2009-12-17 Herbert Sixta Process For Producing A Pulp
CN102427867A (en) * 2009-05-14 2012-04-25 韦尔豪泽Nr公司 Fibrillated blend of lyocell low DP pulp
TW201938591A (en) * 2018-03-06 2019-10-01 奧地利商蘭仁股份有限公司 Dissolving pulp
WO2021006798A1 (en) * 2019-07-05 2021-01-14 Kiram Ab Method for dissolving pulp from recycled textile material
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1844501A (en) * 2006-05-08 2006-10-11 宜宾丝丽雅股份有限公司 Wood hemp composite cellulose pulp and method for producing same
US20090312536A1 (en) * 2006-05-10 2009-12-17 Herbert Sixta Process For Producing A Pulp
JP2009213389A (en) * 2008-03-10 2009-09-24 Nippon Paper Chemicals Co Ltd System for producing bioethanol using lignocellulose as raw material
CN102427867A (en) * 2009-05-14 2012-04-25 韦尔豪泽Nr公司 Fibrillated blend of lyocell low DP pulp
TW201938591A (en) * 2018-03-06 2019-10-01 奧地利商蘭仁股份有限公司 Dissolving pulp
WO2021006798A1 (en) * 2019-07-05 2021-01-14 Kiram Ab Method for dissolving pulp from recycled textile material
CN112853796A (en) * 2021-01-07 2021-05-28 杭州融凯盛科技有限公司 Preparation method for modifying papermaking pulp into pulp special for lyocell fibers

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Title
陈春霞等: "酸性亚硫酸盐与预水解硫酸盐法溶解浆生产工艺及产品性能的比较", 《中国造纸》, vol. 34, no. 12, pages 66 - 70 *

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