CN111320705A - Preparation method of high-viscosity cellulose ether - Google Patents
Preparation method of high-viscosity cellulose ether Download PDFInfo
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- CN111320705A CN111320705A CN202010338049.3A CN202010338049A CN111320705A CN 111320705 A CN111320705 A CN 111320705A CN 202010338049 A CN202010338049 A CN 202010338049A CN 111320705 A CN111320705 A CN 111320705A
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- fiber
- liquid separation
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- 229920003086 cellulose ether Polymers 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 238000010411 cooking Methods 0.000 claims abstract description 61
- 238000004061 bleaching Methods 0.000 claims abstract description 52
- 239000007788 liquid Substances 0.000 claims abstract description 51
- 239000000835 fiber Substances 0.000 claims abstract description 49
- 238000000926 separation method Methods 0.000 claims abstract description 44
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000002657 fibrous material Substances 0.000 claims abstract description 43
- 239000003513 alkali Substances 0.000 claims abstract description 40
- 238000006266 etherification reaction Methods 0.000 claims abstract description 34
- 239000000843 powder Substances 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 22
- 239000002245 particle Substances 0.000 claims abstract description 10
- 238000002791 soaking Methods 0.000 claims abstract description 9
- 230000001502 supplementing effect Effects 0.000 claims abstract description 8
- 239000007844 bleaching agent Substances 0.000 claims abstract description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 65
- 239000000243 solution Substances 0.000 claims description 17
- 239000011259 mixed solution Substances 0.000 claims description 16
- 238000001816 cooling Methods 0.000 claims description 13
- 239000007787 solid Substances 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 9
- 229920000742 Cotton Polymers 0.000 claims description 8
- 239000005708 Sodium hypochlorite Substances 0.000 claims description 8
- 238000010612 desalination reaction Methods 0.000 claims description 8
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- 239000002002 slurry Substances 0.000 claims description 7
- 230000008569 process Effects 0.000 abstract description 12
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 3
- 230000006872 improvement Effects 0.000 abstract description 2
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 19
- 239000001768 carboxy methyl cellulose Substances 0.000 description 19
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 19
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 19
- 239000012071 phase Substances 0.000 description 13
- QBKSWRVVCFFDOT-UHFFFAOYSA-N gossypol Chemical compound CC(C)C1=C(O)C(O)=C(C=O)C2=C(O)C(C=3C(O)=C4C(C=O)=C(O)C(O)=C(C4=CC=3C)C(C)C)=C(C)C=C21 QBKSWRVVCFFDOT-UHFFFAOYSA-N 0.000 description 12
- 238000006243 chemical reaction Methods 0.000 description 10
- 229920002678 cellulose Polymers 0.000 description 7
- 239000001913 cellulose Substances 0.000 description 7
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 6
- QHOPXUFELLHKAS-UHFFFAOYSA-N Thespesin Natural products CC(C)c1c(O)c(O)c2C(O)Oc3c(c(C)cc1c23)-c1c2OC(O)c3c(O)c(O)c(C(C)C)c(cc1C)c23 QHOPXUFELLHKAS-UHFFFAOYSA-N 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 6
- 239000000460 chlorine Substances 0.000 description 6
- 229910052801 chlorine Inorganic materials 0.000 description 6
- 230000005611 electricity Effects 0.000 description 6
- 229930000755 gossypol Natural products 0.000 description 6
- 229950005277 gossypol Drugs 0.000 description 6
- 238000000227 grinding Methods 0.000 description 6
- 238000005070 sampling Methods 0.000 description 6
- FDRCDNZGSXJAFP-UHFFFAOYSA-M sodium chloroacetate Chemical compound [Na+].[O-]C(=O)CCl FDRCDNZGSXJAFP-UHFFFAOYSA-M 0.000 description 6
- 238000005265 energy consumption Methods 0.000 description 4
- 239000010865 sewage Substances 0.000 description 4
- 239000000428 dust Substances 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 238000010025 steaming Methods 0.000 description 2
- 239000008346 aqueous phase Substances 0.000 description 1
- 238000003339 best practice Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 239000000123 paper Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B11/00—Preparation of cellulose ethers
- C08B11/02—Alkyl or cycloalkyl ethers
- C08B11/04—Alkyl or cycloalkyl ethers with substituted hydrocarbon radicals
- C08B11/10—Alkyl or cycloalkyl ethers with substituted hydrocarbon radicals substituted with acid radicals
- C08B11/12—Alkyl or cycloalkyl ethers with substituted hydrocarbon radicals substituted with acid radicals substituted with carboxylic radicals, e.g. carboxymethylcellulose [CMC]
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06L—DRY-CLEANING, WASHING OR BLEACHING FIBRES, FILAMENTS, THREADS, YARNS, FABRICS, FEATHERS OR MADE-UP FIBROUS GOODS; BLEACHING LEATHER OR FURS
- D06L4/00—Bleaching fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods; Bleaching leather or furs
- D06L4/20—Bleaching fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods; Bleaching leather or furs using agents which contain halogen
- D06L4/22—Bleaching fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods; Bleaching leather or furs using agents which contain halogen using inorganic agents
- D06L4/23—Bleaching fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods; Bleaching leather or furs using agents which contain halogen using inorganic agents using hypohalogenites
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/38—Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic Table
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Materials Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
A preparation method of high-viscosity cellulose ether, belonging to the technical field of fiber processing. The preparation method is characterized by comprising the following preparation steps in sequence: crushing: crushing the fiber material to a particle size of 50-150 meshes; bleaching: supplementing water and a bleaching agent and completing bleaching at 15-75 ℃; after bleaching, carrying out solid-liquid separation to obtain bleached fiber micro powder; and (3) cooking: soaking the fiber micro powder obtained in the step 2) into an alkali liquor with the mass concentration of 1.5-15%, and cooking for 30-90 minutes at the cooking temperature of 150-260 ℃; and etherifying and rinsing to obtain the product. The main improvement of the invention lies in that the whole cellulose ether step sequence is adjusted, and in the production method, the steps of bleaching, cooking, etherification and rinsing adopt the prior process conditions and material ratio of the cellulose ether to obtain ideal preparation effect.
Description
Technical Field
A preparation method of high-viscosity cellulose ether, belonging to the technical field of fiber processing.
Background
Cellulose ether is a high molecular compound which can be dissolved in water, dilute alkali solution and organic solvent, has thermoplasticity and excellent performance, and is widely used in the industries of buildings, cement, petroleum, food, textile, detergent, coating, medicine, paper making, electronic components and the like. The basic steps of a conventional cellulose ether preparation process are: cooking, bleaching, crushing, etherification and rinsing. Wherein the cooking process is to heat the fiber in alkali liquor to over 100 ℃ for reaction; the fiber material after cooking and bleaching is subjected to a crushing process. Wherein the boiled fiber needs to be subjected to multiple operations of temperature rise, rinsing, temperature reduction, liquid removal and the like to avoid the influence of alkali liquor on the bleaching process. The bleached fiber material can avoid the bleaching agent from corroding the crusher, and the operations of heating, rinsing, cooling, removing liquid and the like can be carried out for many times, so that the etherification reaction can be carried out after the crushing.
The inventor of the invention considers that the operations of steaming, bleaching, rinsing, liquid removal and the like which are continuously repeated in the traditional preparation process of the cellulose ether greatly prolong the production process and ensure that the preparation efficiency of the cellulose ether cannot be greatly improved. Moreover, a large amount of alkali-containing sewage and salt-containing sewage are generated in the process; resulting in large dosage of alkali liquor, high energy consumption and high production and sewage treatment costs.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: overcomes the defects of the prior art and provides a preparation method of cellulose ether with low alkali consumption and less sewage.
The technical scheme adopted by the invention for solving the technical problems is as follows: the preparation method of the high-viscosity cellulose ether is characterized by sequentially comprising the following steps:
1) crushing: crushing the fiber material to a particle size of 50-150 meshes;
2) bleaching: supplementing water and a bleaching agent and completing bleaching at 15-75 ℃; after bleaching, carrying out solid-liquid separation to obtain bleached fiber micro powder;
3) and (3) cooking: soaking the fiber micro powder obtained in the step 2) into an alkali liquor with the mass concentration of 1.5-15%, and cooking for 30-90 minutes at the cooking temperature of 100-260 ℃;
4) etherification: improving the mass concentration of the alkali liquor in the system to 45-70% on the basis of the step 3), adding a solvent and an etherifying agent, and carrying out etherification reaction;
5) rinsing: and after the etherification reaction is finished, carrying out solid-liquid separation to obtain solid and liquid, and rinsing the solid obtained by the solid-liquid separation.
The main improvement of the invention lies in that the whole cellulose ether step sequence is adjusted, and in the production method, the steps of bleaching, cooking, etherification and rinsing adopt the prior process conditions and material ratio of the cellulose ether to obtain ideal preparation effect. Compared with the prior art, the preparation method can obtain the similar product with higher viscosity, thereby achieving the prior effect with less addition amount when in use.
The preparation method of the invention firstly crushes the fiber material into micro powder, because the inventor finds that the fiber material in the micro powder state can be well bleached under the condition of no degumming (the main purpose of the traditional preparation method is to perform degumming before bleaching so as to increase the bleaching effect), and the fiber material in the micro powder state has lower requirements on bleaching conditions and higher bleaching efficiency.
The bleached fiber is cooked again, and the main purpose of the cooking is to further expand and loosen the fiber micro powder, thereby being more beneficial to the efficient and stable operation of etherification reaction. Therefore, the range of the alkali liquor concentration can be larger when the steam boiling is carried out, and the fault tolerance rate is higher. The greater the concentration of alkali lye in a certain range, the more the fibre can be bulked in a shorter time. The concentration of lye is lower during cooking in the conventional process because the alkali in the fiber needs to be rinsed out completely after cooking in the process. Obviously, the greater the lye concentration, the greater the amount of rinse water required. However, the object of the present invention is to cook the fiber fine powder after bleaching, and the alkali liquor concentration is increased to reach the etherification condition by adding alkali or concentrating part of water on the basis of the cooking liquor directly after cooking, so the rinsing cost is not needed to be considered, and the alkali liquor concentration of the cooking can be increased as much as possible without damaging the cellulose.
In addition, because the object of the cooking in the invention is the bleached fiber micropowder, and the cooking only expands and loosens the fiber, the actually needed alkali liquor concentration for achieving the purpose is lower. That is, in the present invention, the cooking can be performed at a lower alkali solution concentration. However, alkali is directly added on the basis of the cooking liquor after cooking to improve the alkali liquor concentration to reach the etherification condition, no matter the concentration of the cooking liquor is high or low, alkali liquor waste is not caused or the rinsing cost is increased, so that the alkali liquor mass concentration is preferably 10-15% during cooking.
Preferably, the fiber material in the step 1) is cotton linters.
Preferably, the pulverization in the step 1) is to add the fiber material and water into a wet pulverizer simultaneously, and pulverize the fiber material to a particle size of 50-150 meshes to obtain the fiber slurry. The crushing in the invention is preferably carried out by wet crushing, water which is needed in the bleaching process is mixed with the fiber material in advance, the wet crushing is carried out to obtain fiber pulp, and water and bleaching agent are directly supplemented into the fiber pulp to achieve the bleaching concentration. After the wet crushing is adopted, overheating and dust cannot be generated in the crushing process, the noise is lower, the production is safer, no dust pollution exists, and the operation environment is optimized.
In the wet crushing process, the proportion of the fiber material and the water is not a key factor, and the fiber material in a wet state can also achieve the effects of reducing noise, removing dust and the like. The proportion (which can be set between 10:5 and 200) of the fiber materials and water in the crushing in the step 1) is low, and the fault-tolerant capability is high. But in order to increase the fluidity of the slurry, the material transportation cost is reduced. Preferably, the mass ratio of the fiber material to the water in the step 1) is 1: 1.3-6.
In the invention, although the good bleaching effect can be achieved in a wide temperature range. However, in the present invention, the object of bleaching is a fiber fine powder, which has a large specific surface area, and thus bleaching is easily accomplished. The bleaching can be completed at a lower temperature (normal temperature), additional heating is not needed, and the production energy consumption is reduced. Preferably, bleaching is completed in step 2) at 15-25 ℃.
Preferably, the cooking in step 3) is performed by steaming the fiber soaked in the alkali liquor by using a rotary spherical digester.
Preferably, the alkali in the step 4) is NaOH, and the alkali liquor in the steps 3) and 4) is NaOH solution.
Preferably, the water phase of the liquid subjected to solid-liquid separation in the step 5) is directly cooled to-5-10 ℃ after desolventizing, then the solid-liquid separation is carried out to obtain alkali and a mixed solution, and the mixed solution is concentrated and crystallized to realize desalination. In the etherification reaction system, the concentration of alkali in a higher-temperature water phase obtained after desolventizing (the desolventizing comprises distilling to remove an organic solvent and/or an etherifying agent) is higher, the water phase is saturated or nearly saturated, and the concentration of generated salt is lower. At the moment, the aqueous phase is concentrated and crystallized, and the purity of salt in the obtained solid material can reach more than 85 percent without further treatment, so that the purity is greatly improved.
Preferably, the cooking pressure in the step 3) is 0.3 MPa-0.9 MPa. Because cooking in high-concentration lye can be realized in the present preparation method, the required cooking pressure and cooking temperature can be carried out under lower conditions. More preferably, the cooking pressure in the step 3) is 0.3 MPa-0.4 MPa; the cooking temperature is 110-140 ℃.
Preferably, the bleaching agent in step 3) is sodium hypochlorite.
Compared with the prior art, the invention has the beneficial effects that: the preparation method of the invention saves the rinsing process after the cooking, and simultaneously improves the efficiency of each step, thereby greatly improving the overall production efficiency. The production time required for a batch of cellulose ether with the same yield is only 50% -60% of the time required by the traditional preparation method. In addition, in the preparation method, because the reaction conditions of the steps can be carried out under milder conditions, under the conditions of lower temperature and pressure and fewer production links, under the preferable preparation conditions, the energy consumption required by a batch of cellulose ether with the same yield is only 60-70% of the energy consumption required by the traditional preparation method. Meanwhile, compared with the traditional preparation method, the preparation method disclosed by the invention has the advantages that the water consumption is reduced by 30-35%, and the alkali consumption is reduced by 20-30%.
Detailed Description
The present invention is further illustrated by the following specific examples, wherein carboxymethyl cellulose is prepared for comparison between examples and comparative examples, because the present invention is not adjusted for the etherification reaction step, and the reaction raw materials and reaction conditions of the etherification reaction can still follow the conditions of the conventional preparation method. With example 1 being the best practice.
Example 1
1) Crushing: simultaneously adding a fiber material (cotton linter) and water into a wet grinder, grinding the fiber material to the particle size of 150 meshes to obtain fiber slurry, wherein the ratio of the fiber material to the water is 1: 3;
2) bleaching: supplementing water and sodium hypochlorite until the effective chlorine content is 2g/L, wherein the mass ratio of the bleaching solution to the fiber material in the step 1) is 10: 1, bleaching at 22-23 ℃; after bleaching, carrying out solid-liquid separation to obtain bleached fiber micro powder;
3) and (3) cooking: soaking the fiber micro powder obtained in the step 2) into NaOH solution with the mass concentration of 14%, and cooking for 35 minutes at the cooking temperature of 120 ℃ and the cooking pressure of 0.3 MPa;
4) etherification: directly concentrating on the basis of the step 3) to improve the mass concentration of the alkali liquor in the reaction system to 60%, cooling to 23 ℃, adding a solvent and sodium monochloroacetate serving as an etherifying agent with the mass 1.2 times that of the fiber micro powder, and carrying out etherification reaction;
5) rinsing: and after the etherification reaction is finished, carrying out solid-liquid separation, rinsing solid obtained by the solid-liquid separation to obtain carboxymethyl cellulose, directly cooling the water phase obtained by the solid-liquid separation to 0 ℃ after the water phase obtained by the solid-liquid separation is subjected to desolventization, carrying out solid-liquid separation to obtain NaOH and a mixed solution with the purity of 98%, and concentrating and crystallizing the mixed solution to realize desalination. In the present example, the steam consumption for producing one ton of carboxymethyl cellulose is 4.5 tons, the electricity consumption is 1022 degrees, the cellulose yield is 1.35% (calculated by gossypol), the viscosity of the 2% aqueous solution of carboxymethyl cellulose is 4360 mPas by sampling and measuring, and the ash content is 0.89%.
Example 2
1) Crushing: simultaneously adding a fiber material (cotton linter) and water into a wet grinder, grinding the fiber material to obtain a fiber slurry, wherein the ratio of the fiber material to the water is 1: 6;
2) bleaching: supplementing water and sodium hypochlorite until the effective chlorine content is 2.3g/L, wherein the mass ratio of the bleaching solution to the fiber material in the step 1) is 10: 1.1, bleaching is finished at 15-17 ℃; after bleaching, carrying out solid-liquid separation to obtain bleached fiber micro powder;
3) and (3) cooking: soaking the fiber micro powder obtained in the step 2) into NaOH solution with the mass concentration of 15%, and cooking for 30 minutes at the cooking temperature of 110 ℃ and the cooking pressure of 0.3 MPa;
4) etherification: directly concentrating on the basis of the step 3) to improve the mass concentration of the alkali liquor in the reaction system to 50%, cooling to 22 ℃, adding a solvent and sodium monochloroacetate serving as an etherifying agent with the mass 1.1 times that of the fiber micro powder, and carrying out etherification reaction;
5) rinsing: and after the etherification reaction is finished, carrying out solid-liquid separation, rinsing the solid obtained by the solid-liquid separation to obtain carboxymethyl cellulose, directly cooling the water phase obtained by the solid-liquid separation to-5 ℃ after the water phase obtained by the solid-liquid separation is subjected to desolventizing, carrying out solid-liquid separation to obtain NaOH and a mixed solution with the purity of 98.3%, and concentrating and crystallizing the mixed solution to realize desalination. In the present example, the steam consumption for producing one ton of carboxymethyl cellulose is 4.5 tons, the electricity consumption is 1022 degrees, the cellulose yield is 1.35% (calculated by gossypol), the viscosity of the 2% aqueous solution of carboxymethyl cellulose is 4363 mPas by sampling and measuring, and the ash content is 0.91%.
Example 3
1) Crushing: simultaneously adding fiber materials (cotton linters) and water into a wet grinder, grinding the fiber materials to obtain fiber pulp with the particle size of 150 meshes, wherein the ratio of the fiber materials to the water is 1: 1.3;
2) bleaching: supplementing water and sodium hypochlorite until the effective chlorine content is 2.2g/L, wherein the mass ratio of the bleaching solution to the fiber material in the step 1) is 10: 1, bleaching at 20-23 ℃; after bleaching, carrying out solid-liquid separation to obtain bleached fiber micro powder;
3) and (3) cooking: soaking the fiber micro powder obtained in the step 2) into NaOH solution with the mass concentration of 10%, and cooking for 40 minutes at the cooking temperature of 140 ℃ and the cooking pressure of 0.5 MPa;
4) etherification: directly adding NaOH to improve the mass concentration of the alkali liquor in the reaction system to 65% on the basis of the step 3), cooling to 20 ℃, adding an etherifying agent sodium monochloroacetate of which the mass is 1.3 times that of the solvent and the fiber micro powder, and carrying out etherification reaction;
5) rinsing: and after the etherification reaction is finished, carrying out solid-liquid separation, rinsing the solid obtained by the solid-liquid separation to obtain carboxymethyl cellulose, directly cooling the water phase obtained by the solid-liquid separation to 5 ℃, carrying out solid-liquid separation to obtain NaOH and a mixed solution with the purity of 98.1%, and concentrating and crystallizing the mixed solution to realize desalination. In this example, the steam consumption for each ton of carboxymethyl cellulose is 4.4 tons, the electricity consumption is 1021 degrees, the cellulose yield is 1.34% (calculated by gossypol), and the viscosity of the obtained 2% aqueous solution of carboxymethyl cellulose is 4357 mPas by sampling and measuring, and the ash content is 1.2%.
Example 4
1) Crushing: simultaneously adding a fiber material (cotton linter) and water into a wet grinder, grinding the fiber material to obtain a fiber slurry with the particle size of 50 meshes, wherein the ratio of the fiber material to the water is 10: 5;
2) bleaching: supplementing water and sodium hypochlorite until the effective chlorine content is 2.8g/L, wherein the mass ratio of the bleaching solution to the fiber material in the step 1) is 10: 1, completing bleaching at 75 ℃; after bleaching, carrying out solid-liquid separation to obtain bleached fiber micro powder;
3) and (3) cooking: soaking the fiber micro powder obtained in the step 2) into NaOH solution with the mass concentration of 1.5%, and cooking for 90 minutes at the cooking temperature of 260 ℃ and the cooking pressure of 0.9 MPa;
4) etherification: directly adding NaOH to improve the mass concentration of the alkali liquor in the reaction system to 45% on the basis of the step 3), cooling to 50 ℃, adding an etherifying agent sodium monochloroacetate of which the mass is 1.0 time that of the solvent and the fiber micro powder, and carrying out etherification reaction;
5) rinsing: and after the etherification reaction is finished, carrying out solid-liquid separation, rinsing solid obtained by the solid-liquid separation to obtain carboxymethyl cellulose, directly cooling water phase obtained by the solid-liquid separation to 10 ℃ and carrying out solid-liquid separation to obtain NaOH and a mixed solution with the purity of 99%, and concentrating and crystallizing the mixed solution to realize desalination. In this example, the steam consumption for each ton of carboxymethyl cellulose is 4.8 tons, the electricity consumption is 1023 degrees, the cellulose yield is 1.35% (calculated by gossypol), and the viscosity of the obtained 2% aqueous solution of carboxymethyl cellulose is 4257 mPas by sampling and the ash content is 1.2%.
Example 5
1) Crushing: simultaneously adding fiber materials (cotton linters) and water into a wet grinder, grinding the fiber materials to a particle size of 66 meshes to obtain fiber slurry, wherein the ratio of the fiber materials to the water is 10: 200;
2) bleaching: supplementing water and sodium hypochlorite until the effective chlorine content is 3g/L, wherein the mass ratio of the bleaching solution to the fiber material in the step 1) is 10: 2, completing bleaching at 65 ℃; after bleaching, carrying out solid-liquid separation to obtain bleached fiber micro powder;
3) and (3) cooking: soaking the fiber micro powder obtained in the step 2) into NaOH solution with the mass concentration of 2%, and cooking for 85 minutes at the cooking temperature of 240 ℃ and the cooking pressure of 0.8 MPa;
4) etherification: directly adding NaOH to improve the mass concentration of the alkali liquor in the reaction system to 70% on the basis of the step 3), cooling to 45 ℃, adding an etherifying agent sodium monochloroacetate of which the mass is 1.2 times that of the solvent and the fiber micro powder, and carrying out etherification reaction;
5) rinsing: and after the etherification reaction is finished, carrying out solid-liquid separation, rinsing solid obtained by the solid-liquid separation to obtain carboxymethyl cellulose, directly cooling the water phase obtained by the solid-liquid separation to 0 ℃ after the water phase obtained by the solid-liquid separation is subjected to desolventization, carrying out solid-liquid separation to obtain NaOH and a mixed solution with the purity of 98%, and concentrating and crystallizing the mixed solution to realize desalination. In the present example, the steam consumption for producing one ton of carboxymethyl cellulose is 4.7 tons, the electricity consumption is 1022 ℃, the cellulose yield is 1.35% (calculated by gossypol), and the viscosity of the 2% aqueous solution of the carboxymethyl cellulose is 4236 mPas by sampling and the ash content is 1.1%.
Example 6
1) Crushing: putting a fiber material (cotton linter) into a dry-method grinder, and grinding the fiber material to obtain fiber powder with the particle size of 50-150 meshes;
2) bleaching: adding water and sodium hypochlorite into the fiber powder until the effective chlorine content is 2.5g/L, wherein the mass ratio of the bleaching solution to the fiber material in the step 1) is 10: 1, completing bleaching at 45 ℃; after bleaching, carrying out solid-liquid separation to obtain bleached fiber micro powder;
3) and (3) cooking: soaking the fiber micro powder obtained in the step 2) into NaOH solution with the mass concentration of 6%, and cooking for 50 minutes at the cooking temperature of 160 ℃ and the cooking pressure of 0.4 MPa;
4) etherification: directly adding NaOH to improve the mass concentration of the alkali liquor in the reaction system to 55% on the basis of the step 3), cooling to 30 ℃, adding an etherifying agent sodium monochloroacetate of which the mass is 1.1 times that of the solvent and the fiber micro powder, and carrying out etherification reaction;
5) rinsing: and after the etherification reaction is finished, carrying out solid-liquid separation, rinsing solid obtained by the solid-liquid separation to obtain carboxymethyl cellulose, directly cooling a water phase obtained by the solid-liquid separation to-5-10 ℃ after the water phase obtained by the solid-liquid separation is subjected to desolventizing to obtain alkali and a mixed solution, and concentrating and crystallizing the mixed solution to realize desalination. In the present example, the steam consumption for producing one ton of carboxymethyl cellulose is 4.6 tons, the electricity consumption is 1028 ℃, the cellulose yield is 1.35% (calculated by gossypol), and the viscosity of the 2% aqueous solution of the obtained carboxymethyl cellulose is 4151 mPas by sampling and measuring, and the ash content is 1.1%.
The foregoing is directed to preferred embodiments of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the protection scope of the technical solution of the present invention.
Claims (10)
1. The preparation method of the high-viscosity cellulose ether is characterized by sequentially comprising the following steps:
1) crushing: crushing the fiber material to a particle size of 50-150 meshes;
2) bleaching: supplementing water and a bleaching agent and completing bleaching at 15-75 ℃; after bleaching, carrying out solid-liquid separation to obtain bleached fiber micro powder;
3) and (3) cooking: soaking the fiber micro powder obtained in the step 2) into an alkali liquor with the mass concentration of 1.5-15%, and cooking for 30-90 minutes at the cooking temperature of 100-260 ℃;
4) etherification: improving the mass concentration of the alkali liquor in the system to 45-70% on the basis of the step 3), adding a solvent and an etherifying agent, and carrying out etherification reaction;
5) rinsing: and after the etherification reaction is finished, carrying out solid-liquid separation to obtain solid and liquid, and rinsing the solid obtained by the solid-liquid separation.
2. The method for preparing high-viscosity cellulose ether according to claim 1, wherein: the fiber material in the step 1) is cotton linter.
3. The method for preparing high-viscosity cellulose ether according to claim 1, wherein: the crushing in the step 1) is to add the fiber material and water into a wet crusher at the same time, and crush the fiber material to obtain the fiber slurry with the particle size of 50-150 meshes.
4. The method for preparing high-viscosity cellulose ether according to claim 3, wherein: the mass ratio of the fiber material to the water in the step 1) is 1: 3-6.
5. The method for preparing high-viscosity cellulose ether according to claim 1, wherein: bleaching is completed at 15-25 ℃ in the step 2).
6. The method for preparing high-viscosity cellulose ether according to claim 1, wherein: the cooking in the step 3) is performed on the fibers soaked in the alkali liquor through a spherical digester.
7. The method for preparing high-viscosity cellulose ether according to claim 1, wherein: the alkali in the step 4) is NaOH, and the alkali liquor in the step 3) and the step 4) is NaOH solution.
8. The method for preparing high-viscosity cellulose ether according to claim 1, wherein: directly cooling the water phase after the liquid subjected to solid-liquid separation in the step 5) is desolventized to-5-10 ℃, then carrying out solid-liquid separation to obtain alkali and a mixed solution, and concentrating and crystallizing the mixed solution to realize desalination.
9. The method for preparing high-viscosity cellulose ether according to claim 1, wherein: the cooking pressure in the step 3) is 0.3 MPa-0.9 MPa.
10. The method for preparing high-viscosity cellulose ether according to claim 1, wherein: the bleaching agent in the step 3) is sodium hypochlorite.
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