CN106084069A - Sodium carboxymethyl cellulose and preparation method thereof - Google Patents
Sodium carboxymethyl cellulose and preparation method thereof Download PDFInfo
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- C08B11/12—Alkyl or cycloalkyl ethers with substituted hydrocarbon radicals substituted with acid radicals substituted with carboxylic radicals, e.g. carboxymethylcellulose [CMC]
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Abstract
The present invention relates to a kind of sodium carboxymethyl cellulose and preparation method thereof, solve existing sodium carboxymethyl cellulose complex process, problem that properties of product have much room for improvement.Technical scheme includes pretreatment, alkalizes, is etherified, ripening, neutralizes, washs and baking step, in described pre-treatment step, cellulose powder after pulverizing, catalyst are put into after fully mixing in isopropanol and are obtained premixed liquid, and three's mass ratio is catalyst: cellulose powder: isopropanol is (0.1 0.01): 1:(10 25).The inventive method technique is simple, production cost is low, environmentally friendly, the sodium carboxymethyl cellulose of preparation has high molecular, high substituted degree, a high viscosity, and property indices is excellent.
Description
Technical field
The present invention relates to a kind of sodium carboxymethyl cellulose and preparation method thereof.
Background technology
Carboxymethyl cellulose (sodium carboxymethyl cellulose, CMC), is by natural by chemical method
Cellulose be modified and the multifunctional macromolecule compound that obtains, be widely used in the fields such as food, medicine, weaving
In, there is the title of " industry monosodium glutamate ".CMC is dissolved in water can be obviously enhanced the viscosity of solution, has thickening, dispersion, emulsifying, protecting colloid
Etc. excellent effect.Currently, CMC is frequently with hydrophily method and solvent method in production, and the former equipment is simple, but water is difficult to heat conduction and water
In the poor permeability within cellulose, causing etherification procedure insufficient, finally obtained CMC product is of poor quality, salinity and
Water content is the highest；And the CMC of high-quality all uses solvent method to prepare both at home and abroad, organic solvent heat and mass is fast, side reaction
Few, with short production cycle, product quality is high.But, the two main body operation is all that cellulose alkalization, then alkali cellulose carry out ether
Change, last subsequent treatment.Primary raw material is cellulosic material, catalyst, basifier, etherifying agent etc..
CN104371029A discloses a kind of superelevation and glues the preparation method of cross-linking sodium carboxymethyl cellulose, mainly includes alkalization
Reaction, pre-reaction and etherification reaction, wherein pre-reaction includes preliminary etherification reaction and cross-linking reaction, and the two is to occur simultaneously
, contribute to generating the cross-linking sodium carboxymethyl cellulose that etherification reaction replaces uniformly and molecular weight is big, make the viscosity of product obtain
Significantly improve, substitution value about 0.9 time, use the viscosity of Brookfield viscosity meter 1%Na-CMC aqueous solution
Reach 10000cps, improve 40～50% than the viscosity of existing sodium carboxymethyl cellulose.
CN103755816A discloses the preparation method of a kind of sodium carboxymethyl cellulose.It is half by organic solvent
Dry way process prepares sodium carboxymethyl cellulose, with wood pulp or paper pulp as raw material, including: quaternization: by raw material with water for being situated between
Matter and sodium hydroxide carry out quaternization and obtain alkali cellulose；Etherification reaction: alkali cellulose and chloroacetic acid are carried out etherificate anti-
Crude sodium carboxymethylcelluloproduct product should be obtained；Neutralize with washing: during crude sodium carboxymethylcelluloproduct product is carried out in the aqueous solution of alcohol
With, and wash in alcohol；Dried: dried by the solid matter obtained, pulverize, to obtain carboxymethyl after process of sieving fine
Dimension element sodium.
Above-mentioned technology from process for there is the problem that product substitution value is on the low side, process conditions are complicated, cost is high,
From the point of view of preparation, its molecular weight, substitution value, viscosity still need to be improved further.
Summary of the invention
The invention aims to solve above-mentioned technical problem, it is provided that one has high molecular, high substituted degree, high viscous
The sodium carboxymethyl cellulose that degree, property indices are excellent.
The present invention also provides for that a kind of technique is simple, production cost is low, the preparation of environment amenable sodium carboxymethyl cellulose
Method.
The inventive method includes pretreatment, alkalizes, is etherified, ripening, neutralizes, washs and baking step, wherein,
In described pre-treatment step, the cellulose powder after pulverizing, catalyst are put into after fully mixing in isopropanol
Obtaining premixed liquid, three's mixing quality ratio is for catalyst: cellulose powder: isopropanol is (0.1～0.01): 1:(10～25),
Described catalyst is 4-butyl ammonium fluoroborate, tetramethyl ammonium hydrogen sulfate, tetrapropyl ammonium iodide, TPC, methoxy
Formylethyl triphenylphosphinebromide, tetrabutyl ammonium fluoride, tetrabutylammonium chloride, Polyethylene Glycol, trityl group phosphonium iodide,
At least one in aminoanisole.
Make premixed liquid heat up and be maintained at 25～45 DEG C, be added dropwise over mass concentration 10～50% sodium hydroxide solution enter
Row quaternization obtains quaternization liquid, and the addition of sodium hydroxide is the 30～70% of cellulose powder quality, described alkalization
Reaction is carried out under inert gas shielding, and the control quaternization time is 0.5～4.5h.
In described etherification step: make quaternization liquid be warming up to 50～70 DEG C, add chloroacetic acid sodium and carry out etherification reaction
Carry out etherification reaction liquid, described chloroacetic acid sodium addition is cellulose powder quality 80 150%, during etherification reaction
Between be 1～5h.
In described maturation stage: make etherification reaction liquid be cooled to room temperature, it is subsequently adding alcoholic solution to soak etherification reaction liquid,
Soak time is 8-16h.
In described neutralization procedure: with acid solution, the reactant liquor after ripening is neutralized, regulate pH to 6～8, then mistake
Filter.
In described maturation stage, described alcoholic solution is methanol, ethanol or isopropanol.
In described neutralization procedure, acid solution be volumetric concentration be the acetic acid aqueous solution of 70～90%.
Sodium carboxymethyl cellulose of the present invention, is prepared from by said method, and its weight average molecular weight is more than or equal to 700,000,2%B
Viscosity is more than or equal to 50,000 mpas, and substitution value is more than or equal to 0.90, and unit mass product chlorinty is less than or equal to 0.2%.
In order to improve the property indices of sodium carboxymethyl cellulose, existing preparation technology is changed by inventor
Enter, as follows: (1) adds catalyst: it is assumed that the crucial measurement of substitution value and detection are dependent on fiber in alkalinization
The formation of element sodium (alkali cellulose) many and few, in etherification procedure (SN2, bimolecular nucleophilic substitution), alkali cellulose is as parent
Core reagent attack etherifying agentCauseMake chloride ion leave away thus obtain carboxymethyl structure.And it is molten for being etherified efficiency major influence factors
Agent, the nucleophilicity (including stability and the concentration of nucleopilic reagent) of nucleopilic reagent, the leaving capability of leaving group.Inventor passes through
Further investigation finds, the ionic bond of alkali cellulose is easily unstable under polar solvent (wherein water, ethanol etc.), and this is also existing
In technology, hydrophily method can not produce the place of the reason of carboxymethyl cellulose with high degree sodium, does not has high substituted degree as guarantee
(abundant alkali cellulose), etherification reaction below is also it is difficult to ensure that obtain the nucleopilic reagent of q.s, and then can not
It is effectively obtained more preferable etherification product.For solving this problem, inventor considers that adding catalyst participates in reaction.Described catalyst
Effectively play stably the effect of alkali cellulose, it is ensured that the nucleopilic reagent amount of follow-up etherification procedure, such effect is previous
Institute is unanticipated so that the substitution value (0.9) of finished product higher than not using the substitution value (0.6) of catalyst, described in urge
Agent is 4-butyl ammonium fluoroborate, tetramethyl ammonium hydrogen sulfate, tetrapropyl ammonium iodide, TPC, methoxycarbonyl base
Ethyltriphenylphosphonium bromide, tetrabutyl ammonium fluoride, tetrabutylammonium chloride, Polyethylene Glycol, trityl group phosphonium iodide, m-aminophenyl
At least one in methyl ether, preferably tetrabutyl ammonium fluoride, tetrabutyl ammonium fluoride；(2) defined catalyst is before alkalinization step
Pre-treatment step in add: at the interpolation catalyst of starting stage, make catalyst fully mix in premixed liquid, not only ensure
Stablizing of alkali cellulose, is cooked basis for follow-up etherificate, and the alkaline solution in course of reaction is difficult to and cellulose body
Contact, available catalyst plays the transmitting effect of material.More preferably it is transported to aqueous slkali react on cellulose, at one stroke two
?.Described catalyst: cellulose powder: the mixing quality of isopropanol is than being (0.1～0.01): 1:(10～25), catalyst
Addition can not be too much, alkalinization too much can be caused too fast, and the inhomogeneities of substitution value is increased, and I haven't seen you for ages excessively reduces alkali
Change speed and the extent of reaction, cause substitution value to reduce.
Further, in alkalinization step, alkaline solution be mass concentration be the sodium hydroxide solution of 10～50%, control
The addition of sodium hydroxide is the 30--70% of cellulose powder quality, and molecular weight cellulose too much can be caused to rupture, and product divides
Son amount reduces, viscosity declines, and crosses that I haven't seen you for ages and make to alkalize insufficient, and product substitution value is the highest.In the presence of a catalyst, described alkali
The change response time is 0.5～4.5h, and long meeting causes viscosity to reduce, and too short meeting causes substitution value to reduce.
Further, after etherification step, have employed maturation stage, the etherification reaction liquid that i.e. will be cooled to room temperature adds alcohol
Solution soaking is to substitute conventional washing step, and the purpose of immersion is to ensure that reaction system preferably reaches salt balance, for
The follow-up salt matter that more washes away provides prerequisite, and controlling soak time is 8～16h, and too short meeting causes salt matter fully not enter
Enter to reactor liquid layer so that final wash difficulty increases.Described alcoholic solution is preferably in methanol, ethanol or isopropanol at least
A kind of.
Further, in described neutralization procedure: with acid solution, the reactant liquor after ripening is neutralized, regulate pH to 6
～8, then filter.Described acid solution can use aqueous hydrochloric acid solution or acetic acid aqueous solution, acetic acid is preferably used water-soluble, this
Bright method uses water-soluble relatively other acid solution of acetic acid be neutralized and will not introduce chloride ion, and volumetric concentration is preferably controlled in
70～90%, too low meeting causes portioned product to hydrolyze, and too high meeting causes N-process the slowest.
Beneficial effect:
Present invention process method is simple, production cost is low, environmentally friendly；The sodium carboxymethyl cellulose weight that the present invention produces
Average molecular weight (Mw) is more than or equal to 700,000, and 2%B viscosity is more than 50,000 mpas (mPa.s), and substitution value is more than or equal to 0.90, and single
Position quality product chlorinty is less than or equal to 0.2%, and properties is excellent.
Accompanying drawing explanation
Fig. 1 is that the sodium carboxymethyl cellulose that obtains of embodiment 1 is at Fourier infrared spectrum.
Detailed description of the invention
Below in embodiment, raw material and specification: cellulosic material (degree of polymerization is 2500-3000), isopropanol (is analyzed
Pure), ethanol (analytical pure), sodium hydroxide (analytical pure), sodium chloroacetate (analytical pure), acetic acid (analytical pure).
Embodiment 1
A kind of high-performance sodium carboxymethyl cellulose of preparation, method comprises the steps:
(1) pretreatment:
A cellulosic material is pulverized machine with Plant fiber and is crushed to 20 microns and obtains cellulose powder by ()；
B isopropanol that 2kg cellulose powder after 20g 4-butyl ammonium fluoroborate and pulverizing is put into 25L by () successively is molten
In liquid, stirring and evenly mixing obtains premixed liquid；Then subsequent reactions is carried out in nitrogen protection；
(2) alkalization:
Premixed liquid is warming up to 25 DEG C, is then added dropwise over the sodium hydroxide solution 9.1L that mass concentration is 10%, reaction
0.5h obtains quaternization liquid；
(3) etherificate:
Quaternization liquid is warming up to 50 DEG C and add 2.4kg chloroacetic acid sodium reaction 2h obtain etherification reaction liquid；
(4) ripening: etherification reaction liquid is naturally cooled to room temperature, is then added in methanol solution soak 8h；
(5) neutralize: being 70% acetic acid by volumetric concentration is neutralized the reactant liquor after aging, regulates pH to 6～8, so
Rear filtration, obtains filtering residue；
(6) washing: with the washing with alcohol filtering residue that volumetric concentration is 70% 5 times；
(7) dry: be dried to obtain carboxymethyl cellulose by completely cutting off air in the filtering residue feeding drying baker after washing 60 DEG C
Sodium, its molecular weight is 77.8 ten thousand, and viscosity is 52415 mpas (mPa.s), and substitution value is 0.91, and chlorinty is 0.18wt%.
The sodium carboxymethyl cellulose obtaining embodiment 1 is analyzed, and does not demonstrates quaternary ammonium in Fourier infrared spectrum
The characteristic peak of salt；See Fig. 1,3500～3300cm-1The stretching vibration of-OH on the peak correspondence CMC strand skeleton at place, 3000～
2800cm-1Peak correspondence CH at place, CH2Stretching vibration；1650～1550cm-1The opposition of-COO-on the peak correspondence CMC molecule at place
Claim and symmetrical stretching vibration；1430～1260cm-1C-H stretching vibration on the peak correspondence CMC carboxymethyl at place；In collection of illustrative plates not
The characteristic peak of quaternary ammonium salt occurs.
Embodiment 2
A kind of high-performance sodium carboxymethyl cellulose of preparation, method comprises the steps:
(1) pretreatment:
A cellulosic material is pulverized machine with Plant fiber and is crushed to 40 microns and obtains cellulose powder by ()；
B isopropanol that 1kg cellulose powder after 20g tetrapropyl ammonium iodide and pulverizing is put into 18.75L by () successively is molten
In liquid, stirring and evenly mixing obtains premixed liquid；Then subsequent reactions is carried out in nitrogen protection；
(2) alkalization:
Premixed liquid is warming up to 30 DEG C, is then added dropwise over the sodium hydroxide solution 1.1L that mass concentration is 35%, reaction
1h obtains quaternization liquid；
(3) etherificate:
Quaternization liquid is warming up to 55 DEG C and add 1.2kg chloroacetic acid sodium reaction 2h obtain etherification reaction liquid；
(4) ripening: etherification reaction liquid is naturally cooled to room temperature, is then added in methanol solution soak 10h；
(5) neutralize: being 75% acetic acid by volumetric concentration is neutralized the reactant liquor after aging, regulates pH to 6～8, so
Rear filtration, obtains filtering residue；
(6) washing: with the washing with alcohol filtering residue that volumetric concentration is 75% 5 times；
(7) dry: be dried to obtain carboxymethyl cellulose by completely cutting off air in the filtering residue feeding drying baker after washing 70 DEG C
Sodium, its molecular weight is 72.6 ten thousand, and viscosity is 51082 mpas (mPa.s), and substitution value is 0.92, and chlorinty is 0.15%.
Embodiment 3
A kind of high-performance sodium carboxymethyl cellulose of preparation, method comprises the steps:
(1) pretreatment:
A cellulosic material is pulverized machine with Plant fiber and is crushed to 60 microns and obtains cellulose powder by ()；
B 3kg cellulose powder after 50g tetrabutyl ammonium fluoride and pulverizing is put into the aqueous isopropanol of 75L by () successively
Middle stirring and evenly mixing obtains premixed liquid；Then subsequent reactions is carried out in nitrogen protection；
(2) alkalization:
Premixed liquid is warming up to 35 DEG C, is then added dropwise over the sodium hydroxide solution 3.9L that mass concentration is 30%, reaction
2h obtains quaternization liquid；
(3) etherificate:
Quaternization liquid is warming up to 55 DEG C and add 3.6kg chloroacetic acid sodium reaction 3h obtain etherification reaction liquid；
(4) ripening: etherification reaction liquid is naturally cooled to room temperature, is then added in methanol solution soak 12h；
(5) neutralize: being 80% acetic acid by volumetric concentration is neutralized the reactant liquor after aging, regulates pH to 6～8, so
Rear filtration, obtains filtering residue；
(6) washing: with the washing with alcohol filtering residue that volumetric concentration is 80% 5 times；
(7) dry: be dried to obtain carboxymethyl cellulose by completely cutting off air in the filtering residue feeding drying baker after washing 80 DEG C
Sodium, its molecular weight is 73.8 ten thousand, and viscosity is 50046 mpas (mPa.s), and substitution value is 0.93, and chlorinty is 0.13%.
Embodiment 4
A kind of high-performance sodium carboxymethyl cellulose of preparation, method comprises the steps:
(1) pretreatment:
A cellulosic material is pulverized machine with Plant fiber and is crushed to 80 microns and obtains cellulose powder by ()；
B 2.5kg cellulose powder after 125g methoxycarbonyl base ethyltriphenylphosphonium bromide and pulverizing is put into by () successively
In the aqueous isopropanol of 62.5L, stirring and evenly mixing obtains premixed liquid；Then subsequent reactions is carried out in nitrogen protection；
(2) alkalization:
Premixed liquid is warming up to 40 DEG C, is then added dropwise over the sodium hydroxide solution 2.3L that mass concentration is 40%, reaction
3h obtains quaternization liquid；
(3) etherificate:
Quaternization liquid is warming up to 65 DEG C and add 4kg chloroacetic acid sodium reaction 4h obtain etherification reaction liquid；
(4) ripening: etherification reaction liquid is naturally cooled to room temperature, is then added in methanol solution soak 14h；
(5) neutralize: being 85% acetic acid by volumetric concentration is neutralized the reactant liquor after aging, regulates pH to 6～8, so
Rear filtration, obtains filtering residue；
(6) washing: with the washing with alcohol filtering residue that volumetric concentration is 85% 5 times；
(7) dry: be dried to obtain carboxymethyl cellulose by completely cutting off air in the filtering residue feeding drying baker after washing 90 DEG C
Sodium, its molecular weight is 71.6 ten thousand, and viscosity is 50128 mpas (mPa.s), and substitution value is 0.96, and chlorinty is 0.16%.
Embodiment 5
A kind of high-performance sodium carboxymethyl cellulose of preparation, method comprises the steps:
(1) pretreatment:
A cellulosic material is pulverized machine with Plant fiber and is crushed to 100 microns and obtains cellulose powder by ()；
B 5kg cellulose powder after 500g Polyethylene Glycol and pulverizing is put in the aqueous isopropanol of 160L by () successively
Stirring and evenly mixing obtains premixed liquid；Then subsequent reactions is carried out in nitrogen protection；
(2) alkalization:
Premixed liquid is warming up to 45 DEG C, is then added dropwise over the sodium hydroxide solution 4.0L that mass concentration is 45%, reaction
4.5h obtains quaternization liquid；
(3) etherificate:
Quaternization liquid is warming up to 70 DEG C and add 6kg chloroacetic acid sodium reaction 5h obtain etherification reaction liquid；
(4) ripening: etherification reaction liquid is naturally cooled to room temperature, is then added in methanol solution soak 16h；
(5) neutralize: being 90% acetic acid by volumetric concentration is neutralized the reactant liquor after aging, regulates pH to 6～8, so
Rear filtration, obtains filtering residue；
(6) washing: with the washing with alcohol filtering residue that volumetric concentration is 90% 5 times；
(7) dry: be dried to obtain carboxymethyl cellulose by completely cutting off air in the filtering residue feeding drying baker after washing 100 DEG C
Sodium, its molecular weight is 72.9 ten thousand, and viscosity is 51129 mpas (mPa.s), and substitution value is 0.99, and chlorinty is 0.12%.
Comparative example 1
A kind of high-performance sodium carboxymethyl cellulose of preparation, method comprises the steps:
(1) pretreatment:
A cellulosic material is pulverized machine with Plant fiber and is crushed to 60 microns and obtains cellulose powder by ()；
B () puts into the isopropyl of 62.5L successively without any catalyst, the 5kg cellulose powder after directly pulverizing
In alcoholic solution, stirring and evenly mixing obtains premixed liquid；Then subsequent reactions is carried out in nitrogen protection；
(2) alkalization:
Premixed liquid is warming up to 42 DEG C, is then added dropwise over the sodium hydroxide solution 4.3L that mass concentration is 40%, reaction
4.2h obtains quaternization liquid；
(3) etherificate:
Quaternization liquid is warming up to 65 DEG C and add 4.8kg chloroacetic acid sodium reaction 3h obtain etherification reaction liquid；
(4) ripening: etherification reaction liquid is naturally cooled to room temperature, is then added in methanol solution soak 12h；
(5) neutralize: being 90% acetic acid by volumetric concentration is neutralized the reactant liquor after aging, regulates pH to 6～8, so
Rear filtration, obtains filtering residue；
(6) washing: with the washing with alcohol filtering residue that volumetric concentration is 90% 5 times；
(7) dry: be dried to obtain carboxymethyl cellulose by completely cutting off air in the filtering residue feeding drying baker after washing 80 DEG C
Sodium, its molecular weight is 43.2 ten thousand, and viscosity is 20168 mpas (mPa.s), and substitution value is 0.62, and chlorinty is 0.12%.
Comparative example 2
A kind of high-performance sodium carboxymethyl cellulose of preparation, method comprises the steps:
(1) pretreatment:
A cellulosic material is pulverized machine with Plant fiber and is crushed to 100 microns and obtains cellulose powder by ()；
B isopropanol that 4kg cellulose powder after 200g m-Anisidine and pulverizing is put into 100L by () successively is molten
In liquid, stirring and evenly mixing obtains premixed liquid；Then subsequent reactions is carried out in nitrogen protection；
(2) alkalization:
Premixed liquid is warming up to 36 DEG C, is then added dropwise over the sodium hydroxide solution 4.3L that mass concentration is 40%, reaction
3.6h obtains quaternization liquid；
(3) etherificate:
Quaternization liquid is warming up to 60 DEG C and add 4.8kg chloroacetic acid sodium reaction 2.5h obtain etherification reaction liquid；
(4) ripening: etherification reaction liquid is naturally cooled to room temperature；
(5) neutralize: being 70% acetic acid by volumetric concentration is neutralized the reactant liquor after aging, regulates pH to 6～8, so
Rear filtration, obtains filtering residue；
(6) washing: with the washing with alcohol filtering residue that volumetric concentration is 80% 5 times；
(7) dry: be dried to obtain carboxymethyl cellulose by completely cutting off air in the filtering residue feeding drying baker after washing 95 DEG C
Sodium, its molecular weight is 68.6 ten thousand, and viscosity is 56623 mpas (mPa.s), and substitution value is 0.90, and chlorinty is 3.5%.
Claims (8)
1. the preparation method of a sodium carboxymethyl cellulose, it is characterised in that include pretreatment, alkalize, be etherified, ripening, neutralization,
Washing and baking step, wherein,
In described pre-treatment step, the cellulose powder after pulverizing, catalyst are put into after fully mixing in isopropanol and are obtained
Premixed liquid, three's mass ratio is catalyst: cellulose powder: isopropanol is (0.1～0.01): 1:(10～25), described catalysis
Agent is 4-butyl ammonium fluoroborate, tetramethyl ammonium hydrogen sulfate, tetrapropyl ammonium iodide, TPC, methoxycarbonyl base second
Base triphenylphosphinebromide, tetrabutyl ammonium fluoride, tetrabutylammonium chloride, Polyethylene Glycol, trityl group phosphonium iodide, m-aminophenyl first
At least one in ether.
2. the preparation method of sodium carboxymethyl cellulose as claimed in claim 1, it is characterised in that in described alkalinization step, make
Premixed liquid heats up and is maintained at 25～45 DEG C, be added dropwise over mass concentration 10～50% sodium hydroxide solution carry out quaternization
Obtaining quaternization liquid, the addition of sodium hydroxide is the 30～70% of cellulose powder quality, and described quaternization is in inertia
Carrying out under gas shield, the control quaternization time is 0.5～4.5h.
3. the preparation method of sodium carboxymethyl cellulose as claimed in claim 1, it is characterised in that in described etherification step: make
Quaternization liquid is warming up to 50～70 DEG C, and addition chloroacetic acid sodium carries out etherification reaction and carries out etherification reaction liquid, a described chloroethene
Acid sodium addition is cellulose powder quality 80～150%, the etherification reaction time is 1～5h.
4. the preparation method of sodium carboxymethyl cellulose as claimed in claim 1, it is characterised in that in described maturation stage: make
Etherification reaction liquid is cooled to room temperature, is subsequently adding alcoholic solution to soak etherification reaction liquid, and soak time is 8～16h.
5. the preparation method of the sodium carboxymethyl cellulose as described in any one of claim 1-4, it is characterised in that described neutralization walks
In Zhou: with acid solution, the reactant liquor after ripening is neutralized, regulate pH to 6～8, then filter.
6. the preparation method of sodium carboxymethyl cellulose as claimed in claim 4, it is characterised in that in described maturation stage, institute
Stating alcoholic solution is methanol or ethanol.
7. the preparation method of sodium carboxymethyl cellulose as claimed in claim 4, it is characterised in that in described neutralization procedure, acid
Property solution be volumetric concentration be the acetic acid aqueous solution of 70～90%.
8. a sodium carboxymethyl cellulose, it is characterised in that being prepared from by claim 1-7 any one method, its weight average divides
Son amount is more than or equal to 700,000, and 2%B viscosity is more than or equal to 50,000 mpas, and substitution value is more than or equal to 0.90, and unit mass product
Chlorinty is less than or equal to 0.2%.
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| CN110303116A (en) * | 2019-08-11 | 2019-10-08 | 桑超 | A kind of overlay film sand shell mould coating and preparation method thereof |
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| CN110303116A (en) * | 2019-08-11 | 2019-10-08 | 桑超 | A kind of overlay film sand shell mould coating and preparation method thereof |
| CN114773488A (en) * | 2022-05-19 | 2022-07-22 | 浙江三和食品科技有限公司 | Preparation method of high-transparency sodium carboxymethylcellulose |
| CN114773488B (en) * | 2022-05-19 | 2023-02-28 | 浙江三和食品科技有限公司 | Preparation method of high-transparency sodium carboxymethylcellulose |
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