CN114478807A - Raw material processing method and device in viscose fiber production - Google Patents

Raw material processing method and device in viscose fiber production Download PDF

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Publication number
CN114478807A
CN114478807A CN202210068112.5A CN202210068112A CN114478807A CN 114478807 A CN114478807 A CN 114478807A CN 202210068112 A CN202210068112 A CN 202210068112A CN 114478807 A CN114478807 A CN 114478807A
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China
Prior art keywords
pulp
hydrogen peroxide
viscose
raw material
porridge
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CN202210068112.5A
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Chinese (zh)
Inventor
郭新武
冯文军
谢峰
李斌
张璐
罗云刚
吴渊
罗云强
李自光
刘继霞
尚小杰
刘文杰
李洪亮
荣成浩
张旭
赵伟
刘雁茹
杨开通
周晓锋
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Korla Zhongtai Textile Technology Co ltd
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Korla Zhongtai Textile Technology Co ltd
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Priority to CN202210068112.5A priority Critical patent/CN114478807A/en
Publication of CN114478807A publication Critical patent/CN114478807A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B1/00Preparatory treatment of cellulose for making derivatives thereof, e.g. pre-treatment, pre-soaking, activation
    • C08B1/08Alkali cellulose
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B1/00Preparatory treatment of cellulose for making derivatives thereof, e.g. pre-treatment, pre-soaking, activation
    • C08B1/08Alkali cellulose
    • C08B1/10Apparatus for the preparation of alkali cellulose
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B9/00Cellulose xanthate; Viscose
    • 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

Abstract

The invention relates to the technical field of viscose, in particular to a method and a device for processing raw materials in viscose production, wherein the method comprises the following steps: firstly, conveying pulp raw materials into an impregnation barrel, impregnating in 18-25% alkali liquor, and carrying out an alkalization reaction on the pulp and the alkali liquor to obtain alkalized pulp porridge; secondly, conveying the alkalized pulp porridge to an oxygenolysis barrel for oxidative degradation to obtain oxidized pulp porridge; and step three, sending the oxidized pulp porridge obtained in the step two into a squeezer, and squeezing to obtain the alkali cellulose. The invention adopts a dipping-oxidative degradation method to realize the oxidative degradation of chemical fiber pulp and papermaking pulp, and expands the source of the raw materials of viscose fiber. The raw material treatment device in the viscose fiber production has the advantages of good treatment effect, small occupied area, low energy consumption and low maintenance cost.

Description

Raw material processing method and device in viscose fiber production
Technical Field
The invention relates to the technical field of artificial fibers, in particular to a method and a device for processing raw materials in viscose fiber production.
Background
Viscose (Viscose fiber), called Viscose for short, Viscose silk, one of the man-made fibers. The existing process route of the current viscose fiber factory is as follows: pulp raw material-dipping-squeezing-crushing-ageing-cooling-air conveying-weighing-yellowing-filtering-defoaming-spinning. At present, raw materials used by viscose fibers are special raw materials (hereinafter referred to as chemical fiber pulp) specially used for viscose fiber production, and indexes of the chemical fiber pulp need to meet FZ/T51001-2009. The content of alpha-cellulose (alpha-cellulose for short, methyl cellulose) in chemical fiber pulp needs to be over 89% at least according to standard requirements, wherein the content of the lowest methyl cellulose in cotton pulp for viscose filaments is over 95%. The chemical fiber pulp mainly comprises alpha cellulose, contains a small amount of hemicellulose (cellulose with the polymerization degree of less than 200), contains very low contents of pentosan, resin, lignin, ash, iron and the like, and is characterized in that the alpha cellulose has high purity, less impurities, moderate polymerization degree, small distribution range, good reaction performance and good filtering performance. In the prior art, chemical fiber pulp is soaked by sodium hydroxide aqueous solution with the concentration of about 18 percent, so that cellulose is converted into alkali cellulose, hemicellulose in the pulp is dissolved out, and the polymerization degree is partially reduced; and then squeezing to remove redundant alkali liquor, crushing the blocky alkali cellulose on a crusher to form loose floccules, and increasing the surface area to improve the uniformity of the subsequent yellowing reaction. The alkali cellulose undergoes oxidative cleavage by oxygen in the air to decrease the average degree of polymerization, a process called aging. The degree of polymerization degree decrease is related to temperature and time, and the higher the temperature, the faster the degradation, and the longer the degradation. The method comprises the steps of enabling aged alkali cellulose to react with carbon disulfide in a yellowing machine under the condition of vacuum pumping to generate cellulose xanthate, namely yellowing, and aiming at introducing yellow acid groups to cellulose macromolecules, so that on one hand, the space between cellulose can be increased, hydrogen bonds among the macromolecules are further weakened, and on the other hand, due to the fact that the hydrophilicity of the yellow acid groups is in contact with a solvent, strong solvation effect is generated, so that the alkali cellulose which cannot be dissolved in an alkali liquor originally becomes the cellulose xanthate which can be dissolved in water or dilute alkali liquor. Solid cellulose xanthate is dissolved in dilute alkali solution to obtain viscose. The viscose glue is not easy to form due to high viscosity and salt value, and must be placed for a certain time at a certain temperature to be mature, so that the cellulose xanthate in the viscose glue is gradually hydrolyzed and saponified, the esterification degree is reduced, and the viscosity and the stability of the viscose glue on the action of electrolyte are changed. Filtering and defoaming are carried out while ripening, impurities and bubbles in the viscose are removed, finally the viscose is conveyed to spinning through a pipeline, wet spinning forming is carried out in an acid bath, and the obtained cellulose fiber becomes the viscose fiber after washing, desulfurization, bleaching and drying.
According to data, the design capacity of chemical fiber pulp in China is 260 ten thousand t/a, but the actual capacity of the chemical fiber pulp for viscose fiber in China is only about 110 ten thousand t/a in 2020, while the demand of the chemical fiber pulp in China is 437.4 ten thousand tons in 2020, and although the demand is reduced by 5.77% compared with 2019, the capacity of the chemical fiber pulp in China is far from meeting the demand in China, and a large amount of chemical fiber pulp still needs to be solved by import. Compared with chemical fiber pulp, the capacity of domestic papermaking pulp in 2021 year is more than 1900 ten thousand t/a, and the chemical fiber pulp only accounts for less than 5% of the total pulp production capacity. The chemical fiber pulp used in viscose fiber production has high production cost and insufficient supply, while the papermaking pulp is limited by the existing viscose fiber production process and control conditions, and various indexes can not meet the requirements of the existing viscose fiber production and can not be directly applied to the viscose fiber production. The content of the common alpha cellulose in the papermaking pulp is 82-91%, the content of the alpha cellulose is lower than that in the chemical fiber pulp by 4-7%, and the content of hemicellulose, resin, pentosan, ash and the like is higher, thereby far exceeding the use standard of the existing viscose fiber production process for the chemical fiber pulp. And the papermaking pulp has high polymerization degree and is not easy to degrade, and after the pulp is directly added into alkali liquor for dipping according to the existing viscose fiber production process, the generated alkali cellulose can not fully react with carbon disulfide, and a large amount of impurities cause the increase of carbon disulfide side reactions, so that the existing viscose production process can not be met.
Disclosure of Invention
The invention provides a method and a device for processing raw materials in viscose fiber production, which overcome the defects of the prior art and can effectively solve the problem that the existing viscose staple fiber production process cannot be applied to papermaking pulp.
One of the technical schemes of the invention is realized by the following measures: a method for processing raw materials in viscose fiber production comprises the following steps:
firstly, conveying pulp raw materials into an impregnation barrel, impregnating in 18-25% alkali liquor, and carrying out an alkalization reaction on the pulp and the alkali liquor to obtain alkalized pulp porridge; secondly, conveying the alkalized pulp porridge to an oxygenolysis barrel for oxidative degradation to obtain oxidized pulp porridge; and step three, sending the oxidized pulp porridge obtained in the step two into a squeezer, and squeezing to obtain the alkali cellulose.
The following is a further optimization or/and improvement of one of the above-mentioned technical solutions of the invention:
the pulp raw material is chemical fiber pulp or papermaking pulp.
In the first step, the dipping temperature is 40-60 ℃, and the dipping time is 20 min-1 h.
In the second step, oxidative degradation is carried out by adding the required amount of hydrogen peroxide solution to the alkalized slurry.
The oxidative degradation time is 1 to 2 hours.
The concentration of the hydrogen peroxide solution is 20-30%, and the mass ratio of the hydrogen peroxide solution to the pulp raw material is 0.3-6%.
The mass ratio of the hydrogen peroxide solution to the chemical fiber pulp is 0.3-1.5%.
The mass ratio of the hydrogen peroxide solution to the papermaking pulp is 3-6%.
In the third step, the pressure of the pulp tank of the squeezer is 0.02MPa to 0.08 MPa.
The second technical scheme of the invention is realized by the following measures: the device for implementing the raw material processing method in viscose fiber production comprises an impregnation barrel, a hydrogen peroxide storage tank, an oxygen decomposition barrel and a squeezer, wherein a first material conveying pipeline is fixedly communicated between the discharge end of the impregnation barrel and the feed end of the bottom of the oxygen decomposition barrel, a hydrogen peroxide pipeline is fixedly communicated between the first material conveying pipeline and the hydrogen peroxide storage tank, a second material conveying pipeline is fixedly communicated between the discharge end of the top of the oxygen decomposition barrel and the feed end of the squeezer, a stirrer is fixedly installed at the bottom in the oxygen decomposition barrel, and a delivery pump is fixedly installed on the hydrogen peroxide pipeline.
Drawings
FIG. 1 is a schematic process flow diagram of the present invention.
The codes in the figures are respectively: 1 is the steeping vat, 2 is the hydrogen peroxide storage tank, 3 is the oxygen bucket of decomposing, 4 is the squeezer, 5 is first defeated material pipeline, 6 is the hydrogen peroxide pipeline, 7 is the second defeated material pipeline, 8 is the agitator, 9 is the delivery pump.
Detailed Description
The present invention is not limited by the following examples, and specific embodiments may be determined according to the technical solutions and practical situations of the present invention. The various chemical reagents and chemical articles mentioned in the invention are all the chemical reagents and chemical articles which are well known and commonly used in the prior art, unless otherwise specified; the percentages in the invention are mass percentages unless otherwise specified; the solution in the present invention is an aqueous solution in which the solvent is water, for example, a hydrochloric acid solution is an aqueous hydrochloric acid solution, unless otherwise specified; the normal temperature and room temperature in the present invention generally mean a temperature of 15 ℃ to 25 ℃, and are generally defined as 25 ℃.
In the present invention, unless otherwise specified, all the devices and apparatuses used are conventionally known and used in the art.
The invention is further described below with reference to the following examples:
example 1: the raw material processing method in the viscose fiber production comprises the following steps:
firstly, conveying pulp raw materials into an impregnation barrel 1, impregnating in 18-25% alkali liquor, and carrying out an alkalization reaction on pulp and alkali liquor to obtain alkalized pulp porridge;
secondly, conveying the alkalized pulp porridge to an oxygenolysis barrel 3 for oxidative degradation to obtain oxidized pulp porridge;
and step three, sending the oxidized pulp porridge obtained in the step two into a squeezer 4, and squeezing to obtain the alkali cellulose.
The invention adopts a dipping-oxidative degradation method to treat the pulp raw material. Wherein, the oxidative degradation adopts hydrogen peroxide solution to treat the alkalized pulp, so that the alkalized pulp is subjected to oxidative degradation, and after a certain time of reaction, the hydrogen peroxide is consumed completely, so as to obtain the oxidized pulp porridge. In addition, the ammonia-copper viscosity of the alkali cellulose in the oxidized pulp porridge can reach the level (namely, the ammonia-copper viscosity is about 50) consistent with the ammonia-copper viscosity of the alkali cellulose obtained by the traditional process by adjusting the adding amount of the hydrogen peroxide in the oxidative degradation process. The oxidized pulp is then conveyed to a press 4 for pressing to obtain alkali cellulose. The obtained alkali cellulose can be further crushed, cooled, blown, weighed, yellowed, filtered, defoamed and spun by the prior art to finally obtain the viscose fiber.
Example 2: as the optimization of the embodiment, the pulp raw material is chemical fiber pulp or papermaking pulp.
Example 3: as optimization of the above embodiment, in the first step, the dipping temperature is 40 ℃ to 60 ℃, and the dipping time is 20min to 1 h.
Example 4: as an optimization of the above example, in the second step, oxidative degradation is carried out by adding the desired amount of hydrogen peroxide solution to the alkalized mash.
Example 5: as an optimization of the above example, the oxidative degradation time is 1h to 2 h.
Example 6: as optimization of the above embodiment, the concentration of the hydrogen peroxide solution is 20% to 30%, and the mass ratio of the hydrogen peroxide solution to the pulp raw material is 0.3% to 6%.
Example 7: as optimization of the above embodiment, the mass ratio of the hydrogen peroxide solution to the chemical fiber pulp is 0.3% to 1.5%.
Example 8: as optimization of the above embodiment, the mass ratio of the hydrogen peroxide solution to the papermaking pulp is 3% to 6%.
Example 9: as an optimization of the above embodiment, in the third step, the vat pressure of the press 4 is 0.02MPa to 0.08 MPa.
Example 10: the device for implementing the raw material treatment method in viscose fiber production comprises a steeping vat 1, a hydrogen peroxide storage tank 2, an oxygen decomposition vat 3 and a squeezer 4, wherein a first material conveying pipeline 5 is fixedly communicated between the discharge end of the steeping vat 1 and the feed end at the bottom of the oxygen decomposition vat 3, a hydrogen peroxide pipeline 6 is fixedly communicated between the first material conveying pipeline 5 and the hydrogen peroxide storage tank 2, a second material conveying pipeline 7 is fixedly communicated between the discharge end at the top of the oxygen decomposition vat 3 and the feed end of the squeezer 4, a stirrer 8 is fixedly mounted at the bottom in the oxygen decomposition vat 3, and a delivery pump 9 is fixedly mounted on the hydrogen peroxide pipeline 6.
Example 11: the raw material processing method for viscose fiber production comprises the following steps:
firstly, conveying 1030kg of chemical fiber pulp raw material to an impregnation barrel 1, adding 222g/L sodium hydroxide alkali liquor with the concentration of 22.3m, and impregnating for 28min at the temperature of 50 ℃ to obtain alkalized pulp porridge; secondly, conveying the alkalized pulp porridge into an oxygenolysis barrel 3, simultaneously injecting 27.6 percent hydrogen peroxide solution through a hydrogen peroxide pipeline 6, adding 12kg of the alkalized pulp porridge, reacting for 1.0h, and fully oxidizing and degrading to obtain oxidized pulp porridge; and thirdly, sending the oxidized pulp porridge obtained in the second step into a squeezer 4, and squeezing under the pressure of a pulp tank of 0.045MPa to obtain the alkali cellulose.
The obtained alkali cellulose is further crushed, cooled, air-blown, weighed, yellowed, filtered, defoamed and spun by the prior art to finally obtain the viscose fiber. The obtained viscose fiber is subjected to GB/T14463-.
Example 12: the raw material processing method for viscose fiber production comprises the following steps:
step one, conveying 1000kg of papermaking pulp raw materials into an impregnation barrel 1, adding 238g/L sodium hydroxide alkali liquor with the concentration of 238g/L in a step 2m, and soaking for 32min at the temperature of 52 ℃ to obtain alkalized pulp porridge; secondly, conveying the alkalized pulp porridge into an oxygenolysis barrel 3, simultaneously injecting 27.8 percent hydrogen peroxide solution through a hydrogen peroxide pipeline 6, adding 55kg of the alkalized pulp porridge, reacting for 1.25h, and fully oxidizing and degrading to obtain oxidized pulp porridge; and thirdly, sending the oxidized pulp porridge obtained in the second step into a squeezer 4, and squeezing under the pressure of a pulp tank of 0.050MPa to obtain the alkali cellulose.
The obtained alkali cellulose is further crushed, cooled, air-blown, weighed, yellowed, filtered, defoamed and spun by the prior art to finally obtain the viscose fiber. The obtained viscose fiber is subjected to GB/T14463-.
The invention adopts a dipping-oxidative degradation method to treat the pulp raw material, and can realize the oxidative degradation of chemical fiber pulp and papermaking pulp. In the method, the oxygen decomposition barrel 3 is used for prolonging the time of oxidative degradation of pulp raw materials in alkali liquor, the plant cell walls of paper pulp of the paper pulp are damaged in a high-oxygen and high-alkali environment, the degree of polymerization of fibers is reduced, the characteristics of cellulose are changed, hemicellulose and pentosan are dissolved out, the reaction performance of the pulp is improved, the alkali cellulose with standard and stable performance is produced, and finally the viscose fiber meeting the requirements is produced. The invention realizes the direct production of viscose fiber by the papermaking pulp, and the produced viscose fiber product meets the product quality requirement of the national standard GB/T14463-2008 viscose staple fiber.
Table 2 shows the comparison of the oxidative degradation process with the aging box process and the aging drum process. As can be seen from Table 2, the oxidative degradation process adopted by the invention can shorten the preparation time of the alkali cellulose during the production of the viscose staple fibers by more than 3h, and in addition, the raw material processing device in the production of the viscose staple fibers has the characteristics of small occupied area, low energy consumption and low maintenance cost. In actual production, the treatment method can be used for dismantling the existing ageing system, and can also be used for crushing the obtained alkali cellulose according to requirements and then further carrying out subsequent processes such as ageing, cooling and the like.
In conclusion, the method adopts the dipping-oxidative degradation method to realize the oxidative degradation of the chemical fiber pulp and the papermaking pulp, and expands the sources of the raw materials of the viscose fiber. The raw material treatment device in the viscose fiber production has the advantages of good treatment effect, small occupied area, low energy consumption and low maintenance cost.
The technical characteristics form an embodiment of the invention, which has strong adaptability and implementation effect, and unnecessary technical characteristics can be increased or decreased according to actual needs to meet the requirements of different situations.
Figure 924492DEST_PATH_IMAGE001

Claims (10)

1. A method for processing raw materials in viscose fiber production is characterized by comprising the following steps: firstly, conveying pulp raw materials into an impregnation barrel, impregnating in 18-25% alkali liquor, and carrying out an alkalization reaction on the pulp and the alkali liquor to obtain alkalized pulp porridge; secondly, conveying the alkalized pulp porridge to an oxygenolysis barrel for oxidative degradation to obtain oxidized pulp porridge; and step three, sending the oxidized pulp porridge obtained in the step two into a squeezer, and squeezing to obtain the alkali cellulose.
2. The method for processing raw materials in viscose fiber production according to claim 1, wherein the pulp raw material is chemical fiber pulp or papermaking pulp.
3. The method for processing raw materials in viscose fiber production according to claim 1 or 2, wherein in the first step, the dipping temperature is 40 ℃ to 60 ℃ and the dipping time is 20min to 1 h.
4. A method for the treatment of raw materials in the production of viscose fibres according to any one of claims 1 to 3, characterised in that in the second step the oxidative degradation is carried out by adding a desired amount of hydrogen peroxide solution to the alkalized pulp-gruel.
5. A method for treating raw material in viscose manufacture according to any of claims 1 to 4 characterised in that the oxidative degradation time is 1 to 2 h.
6. The method for treating raw material in viscose fiber production according to any of claims 1 to 5, wherein the concentration of hydrogen peroxide solution is 20% to 30%, and the mass ratio of hydrogen peroxide solution to pulp raw material is 0.3% to 6%.
7. The method of claim 6, wherein the mass ratio of the hydrogen peroxide solution to the chemical fiber pulp is 0.3-1.5%.
8. The method of claim 6, wherein the mass ratio of the hydrogen peroxide solution to the papermaking pulp is 3-6%.
9. The method for treating raw material in viscose fiber production according to any of claims 1 to 8, wherein in the third step, the vat pressure of the press is 0.02MPa to 0.08 MPa.
10. An apparatus for implementing the method of processing raw material in viscose fiber production according to any one of claims 1 to 8, comprising an impregnation tank, a hydrogen peroxide storage tank, an oxygen decomposition tank, and a presser, wherein a first material conveying pipeline is fixedly communicated between the discharge end of the impregnation tank and the feed end of the bottom of the oxygen decomposition tank, a hydrogen peroxide pipeline is fixedly communicated between the first material conveying pipeline and the hydrogen peroxide storage tank, a second material conveying pipeline is fixedly communicated between the discharge end of the top of the oxygen decomposition tank and the feed end of the presser, a stirrer is fixedly installed at the bottom of the oxygen decomposition tank, and a delivery pump is fixedly installed on the hydrogen peroxide pipeline.
CN202210068112.5A 2022-01-20 2022-01-20 Raw material processing method and device in viscose fiber production Pending CN114478807A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN201236223Y (en) * 2008-06-10 2009-05-13 宜宾海丝特纤维有限责任公司 Alkali fiber production apparatus with plant fiber as raw material
CN101603210A (en) * 2008-06-10 2009-12-16 宜宾海丝特纤维有限责任公司 String is made the production method of viscose

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN201236223Y (en) * 2008-06-10 2009-05-13 宜宾海丝特纤维有限责任公司 Alkali fiber production apparatus with plant fiber as raw material
CN101603210A (en) * 2008-06-10 2009-12-16 宜宾海丝特纤维有限责任公司 String is made the production method of viscose

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
杨之礼等: "《纤维素与粘胶纤维 中册》", 31 August 1981, 纺织工业出版社 *
白伦主编: "《纺织工业出版社》", 31 August 2018, 东华大学出版社 *

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