CN110214932A - A kind of high temperature resistant sodium carboxymethylcellulose and preparation method thereof - Google Patents
A kind of high temperature resistant sodium carboxymethylcellulose and preparation method thereof Download PDFInfo
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- CN110214932A CN110214932A CN201910503166.8A CN201910503166A CN110214932A CN 110214932 A CN110214932 A CN 110214932A CN 201910503166 A CN201910503166 A CN 201910503166A CN 110214932 A CN110214932 A CN 110214932A
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- preparation
- solid
- sodium carboxymethylcellulose
- high temperature
- temperature resistant
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- 239000001768 carboxy methyl cellulose Substances 0.000 title claims abstract description 55
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 title claims abstract description 45
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000007787 solid Substances 0.000 claims abstract description 45
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000002994 raw material Substances 0.000 claims abstract description 18
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229920002678 cellulose Polymers 0.000 claims abstract description 10
- 239000001913 cellulose Substances 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 10
- 239000003292 glue Substances 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 8
- 239000012298 atmosphere Substances 0.000 claims abstract description 6
- 239000011812 mixed powder Substances 0.000 claims abstract description 5
- 238000001914 filtration Methods 0.000 claims abstract description 3
- 239000007864 aqueous solution Substances 0.000 claims description 40
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 20
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 12
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 12
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 11
- 229910052786 argon Inorganic materials 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 8
- 238000006386 neutralization reaction Methods 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 239000011261 inert gas Substances 0.000 claims description 6
- 229920000609 methyl cellulose Polymers 0.000 claims description 5
- 239000001923 methylcellulose Substances 0.000 claims description 5
- 239000001307 helium Substances 0.000 claims description 4
- 229910052734 helium Inorganic materials 0.000 claims description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 4
- -1 is neutralized Substances 0.000 claims description 4
- 238000007872 degassing Methods 0.000 claims description 3
- 239000012300 argon atmosphere Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 230000018044 dehydration Effects 0.000 abstract description 5
- 238000006297 dehydration reaction Methods 0.000 abstract description 5
- 235000013305 food Nutrition 0.000 description 16
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 13
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 12
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 12
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 11
- 229940105329 carboxymethylcellulose Drugs 0.000 description 11
- 229920000168 Microcrystalline cellulose Polymers 0.000 description 10
- 239000008186 active pharmaceutical agent Substances 0.000 description 10
- 235000019813 microcrystalline cellulose Nutrition 0.000 description 10
- 239000000203 mixture Substances 0.000 description 10
- 239000011734 sodium Substances 0.000 description 10
- 238000003756 stirring Methods 0.000 description 10
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 7
- 239000001103 potassium chloride Substances 0.000 description 7
- 235000011164 potassium chloride Nutrition 0.000 description 7
- 229910001415 sodium ion Inorganic materials 0.000 description 7
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 description 6
- 229940016286 microcrystalline cellulose Drugs 0.000 description 6
- 239000008108 microcrystalline cellulose Substances 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 6
- 239000003513 alkali Substances 0.000 description 5
- 239000002585 base Substances 0.000 description 5
- 235000010980 cellulose Nutrition 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 230000001376 precipitating effect Effects 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 4
- 239000000654 additive Substances 0.000 description 4
- 230000000996 additive effect Effects 0.000 description 4
- 238000013019 agitation Methods 0.000 description 4
- 230000036541 health Effects 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 229940063834 carboxymethylcellulose sodium Drugs 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 229920003123 carboxymethyl cellulose sodium Polymers 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 description 1
- 229920001817 Agar Polymers 0.000 description 1
- 241001474374 Blennius Species 0.000 description 1
- 208000024172 Cardiovascular disease Diseases 0.000 description 1
- 108010010803 Gelatin Proteins 0.000 description 1
- 206010020772 Hypertension Diseases 0.000 description 1
- 239000008272 agar Substances 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 235000013365 dairy product Nutrition 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 206010012601 diabetes mellitus Diseases 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- PXEDJBXQKAGXNJ-QTNFYWBSSA-L disodium L-glutamate Chemical compound [Na+].[Na+].[O-]C(=O)[C@@H](N)CCC([O-])=O PXEDJBXQKAGXNJ-QTNFYWBSSA-L 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 239000008273 gelatin Substances 0.000 description 1
- 229920000159 gelatin Polymers 0.000 description 1
- 235000019322 gelatine Nutrition 0.000 description 1
- 235000011852 gelatine desserts Nutrition 0.000 description 1
- 235000015243 ice cream Nutrition 0.000 description 1
- 235000008446 instant noodles Nutrition 0.000 description 1
- 235000015110 jellies Nutrition 0.000 description 1
- 239000008274 jelly Substances 0.000 description 1
- 108010079904 microcin Proteins 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 235000013923 monosodium glutamate Nutrition 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000000661 sodium alginate Substances 0.000 description 1
- 235000010413 sodium alginate Nutrition 0.000 description 1
- 229940005550 sodium alginate Drugs 0.000 description 1
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 description 1
- 235000010234 sodium benzoate Nutrition 0.000 description 1
- 239000004299 sodium benzoate Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 229940073490 sodium glutamate Drugs 0.000 description 1
- 235000013555 soy sauce Nutrition 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/015—Inorganic compounds
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/30—Foods or foodstuffs containing additives; Preparation or treatment thereof containing carbohydrate syrups; containing sugars; containing sugar alcohols, e.g. xylitol; containing starch hydrolysates, e.g. dextrin
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Food Science & Technology (AREA)
- Nutrition Science (AREA)
- Engineering & Computer Science (AREA)
- Polymers & Plastics (AREA)
- Molecular Biology (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Jellies, Jams, And Syrups (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
- General Preparation And Processing Of Foods (AREA)
Abstract
The invention discloses a kind of high temperature resistant sodium carboxymethylcelluloses and preparation method thereof.This method comprises: sodium carboxymethylcellulose is mixed with cellulose base foodstuff glue, mixed raw material is obtained, is then de-gassed, is mixed with sulfuric acid solution, isothermal holding, filtering takes filter residue；Filter residue is washed with water, the solid after being washed；Under an inert atmosphere, the solid after washing is added in alkaline mixed-powder, is neutralized, the solid after being neutralized；Dehydration, drying, crushing obtain the high temperature resistant sodium carboxymethylcellulose.Preparation method provided by the invention, method is simple, step is few, and quality is stablized between production batch, not high to equipment requirement, is able to achieve production in existing equipment, obtained high temperature resistant sodium carboxymethylcellulose performance is good, high-temperature viscosity is high.
Description
Technical field
The invention belongs to food additives fields, and in particular to a kind of high temperature resistant sodium carboxymethylcellulose and its preparation side
Method.
Background technique
Sodium carboxymethylcellulose (CMC) uses in food as additive, has thickening, suspends, emulsification, stablize, protect
The multiple functions such as shape, film forming, extruding, anti-corrosive fresh-keeping, acidproof and health care, simultaneously because the price of CMC is compared with gelatin, agar, seaweed
The foodstuff glues such as sour sodium are cheap, be therefore widely used in the beverage of modern food industry, dairy produce, ice cream, soy sauce, jelly,
In the food such as jam, instant noodles.Standard GB/T 2760-2014 is classified as: can be needed in varieties of food items by production appropriate
The additive list (A3,53) used, this means that in food production, and CMC can be added largely.However, research has shown that,
The diseases such as diabetes, hypertension, cardiovascular disease all excessively have close contact with sodium ion intake.
Human body not only by salt take in sodium ion, additive (such as sodium benzoate, sodium glutamate, sodium carboxymethylcellulose,
Sodium alginate etc.) equally also it is absorbed by the human body containing a large amount of sodium ion.Exactly because it is noted that in food processing process
In, additive can also bring a certain amount of sodium ion into.Chinese NNFA, British Food Standards Agency Deng Duojia authoritative institution are recommended
Salt health dose is about 6g/ days, and World Health Organization's recent proposals: adult eating salt amount is changed to 5g by 6g daily.It reduces
The total amount of human body intake sodium ion.On the one hand the intake of appropriate drop high temperature resistant salt, effective method are to increase food
The amount of middle sylvite, to reduce the total amount of sodium ion in human body.It is exactly to add as all occurred the product of high temperature resistant salt in the market
A certain amount of potassium chloride replaces the salt of sodium chloride.
CN201010299707.9 provides a kind of production method of low sodium carboxymethyl cellulose sodium, and there are high-temperature viscosities substantially
The technical issues of degree decline.
Summary of the invention
In order to overcome deficiencies of the prior art, the object of the present invention is to provide a kind of high temperature resistant carboxymethyl celluloses
Plain sodium and preparation method thereof.Preparation method provided by the invention is a kind of resistance to height that quality at low cost, high-efficient, product is high
The production method of warm sodium carboxymethylcellulose.The present invention can be effectively solved the product high-temperature viscosity of prior art production substantially
Degree decline this problem, increases the kind of CMC product, expands its use scope, and reduce the content of its sodium ion, to people
Body health has healthcare function, keeps the sustainable fast-developing with important and profound significance of CMC industry.
The purpose of the present invention is realized at least through one of following technical solution.
A kind of preparation method of high temperature resistant sodium carboxymethylcellulose, includes the following steps:
(1) sodium carboxymethylcellulose (food-grade) is mixed with cellulose base foodstuff glue, obtains mixed raw material, then carries out
Degassing process (inert gas shielding processing), (mass percent concentration is the H of 10-40% with sulfuric acid solution2SO4Aqueous solution) it is mixed
It closes, isothermal holding, filtering takes filter residue；
(2) step (1) described filter residue, the solid after being washed is washed with water；
(3) under an inert atmosphere, the solid after step (2) described washing is added in alkaline mixed-powder, is neutralized
Processing, the solid after being neutralized；
(4) solid after neutralization is dehydrated, drying, crushing obtains the high temperature resistant sodium carboxymethylcellulose.
Further, step (1) the cellulose base foodstuff glue includes microcrystalline cellulose, methylcellulose and hydroxypropyl grade first
Base cellulose；The mass ratio of the sodium carboxymethylcellulose and cellulose base foodstuff glue is 86-99.5:0.5-14.
Further, step (1) described degassing process is deaerated 5-20 minutes in the case where vacuum degree is 0.05-0.10MPa, is filled
Enter inert gas；The inert gas is nitrogen, helium or argon gas.
Further, the mass percent concentration of step (1) described sulfuric acid solution is 10wt%-40wt%；The sulfuric acid
Solution and the volume mass of mixed raw material ratio are 4-16:1L/kg.
Further, the temperature of step (1) described isothermal holding is 10-40 degrees Celsius, and the time of isothermal holding is 2-10
Hour.
Further, the temperature of step (2) described water is 0-30 degrees Celsius.
Further, the water content of the solid after step (3) described washing is 55-65%.
Further, step (3) inert atmosphere is nitrogen atmosphere, helium atmosphere or argon atmosphere；At the neutralization
The temperature of reason is 25-35 degrees Celsius, and the time of neutralisation treatment is 1-6 hours.
Further, step (3) the alkaline mixed-powder, according to parts by weight, comprising:
Na2CO385-98 parts；
K2CO31.5-14 part；
(NH4)2CO30.5-1.5 parts.
Further, the pH value of 1% aqueous solution of solid is that 7.5-8 (prepare after neutralizing by solid after step (3) described neutralization
The aqueous solution for being 1% for mass percent concentration, pH value 7.5-8.0).
The present invention provides a kind of high temperature resistant sodium carboxymethylcellulose as made from above-mentioned preparation method.
High temperature resistant sodium carboxymethylcellulose provided by the invention, high temperature (60-65 DEG C) viscosity are greater than in its raw material directly
Stir physical mixed.
Compared with prior art, the invention has the advantages that and the utility model has the advantages that
(1) preparation method provided by the invention, the inert gas shielding technology of use utilize 86-99.5 parts of food-grade carboxylics
Sodium carboxymethylcellulose pyce and 0.5-14 parts of cellulose base foodstuff glues are raw material, obtain high temperature resistant (60-65 DEG C) sodium carboxymethylcellulose,
The stable product quality produced between this method batch, the high temperature resistant sodium carboxymethylcellulose performance produced is high, compared to handle
The method of the direct physical mixed of raw material, viscosity is higher under high temperature resistant sodium carboxymethylcellulose high temperature produced by the present invention.
Specific embodiment
Specific implementation of the invention is described further below in conjunction with example, but implementation and protection of the invention is not limited to
This.If being that those skilled in the art can refer to prior art reality it is noted that there is the process of not special detailed description below
It is existing or understanding.Reagents or instruments used without specified manufacturer, being considered as can be by the commercially available conventional products being commercially available.
Embodiment 1
A kind of preparation method of high temperature resistant sodium carboxymethylcellulose, includes the following steps:
The first step, by food level sodium carboxymethylcellulose (FL20 type, DS=0.92,25 DEG C, 1%wt Aqueous Solution Viscosity
(Brookfield) 40mPa, purity 99.5%) and 55.9g and 9.1g microcrystalline cellulose (MCC25 DEG C, 2%wt Aqueous Solution Viscosity
(Brookfield) 2mPa, purity 99.8%) mixing, it then deaerates 5 minutes in the case where vacuum degree is 0.05MPa, is filled with nitrogen,
The H that mass percent concentration is 10% is added2SO4Aqueous solution 1040mL；
Second step, 10 DEG C keep the temperature 10 hours, centrifuge separation, take precipitating, 0 DEG C of water washing of obtained solid, be centrifugated,
Obtain the solid that water content is 55%wt；
Third step, under nitrogen protection, the water content that second step is obtained are the solid of 55%wt, and 10.7g alkalinity is added
(by Na in mix powder2CO3、K2CO3And (NH4)2CO3Composition；The Na2CO3、K2CO3And (NH4)2CO3Mass ratio be
85:14:1.5)；Alkali: the carboxymethyl in raw material (food level sodium carboxymethylcellulose) is 1:2 (molar ratio), keeps the temperature (temperature 25
DEG C) 6 hours, the solid after being neutralized；If gained neutralize after solid be formulated as mass percent concentration be 1% it is water-soluble
Liquid, pH value 7.5；
4th step, third step is neutralized after solid dehydration, drying, crush, it is fine to obtain the high temperature resistant carboxymethyl
Tie up plain sodium.
The DS=0.90 (Na:0.56, K:0.06) of gained high temperature resistant sodium carboxymethylcellulose, 25 DEG C, 1.0%wt is water-soluble
Liquid viscosity (Brookfield) is 55mPa, purity 99.8%, 60 DEG C of stirrings, 1 hour product 1.0%wt Aqueous Solution Viscosity
(Brookfield) be 35mPa, raw material in proportion CMC, MCC and K (food level sodium carboxymethylcellulose, microcrystalline cellulose and
KCl) the mixture of physical agitation mixing, at 25 DEG C, 1.0% Aqueous Solution Viscosity is (Brookfield) 30mPa, at 60 DEG C,
1.0% Aqueous Solution Viscosity (Brookfield) is 23mPa.
Embodiment 2
A kind of preparation method of high temperature resistant sodium carboxymethylcellulose, includes the following steps:
The first step, by production do not purify food level sodium carboxymethylcellulose (FL100 type, DS=0.92,25 DEG C,
1% Aqueous Solution Viscosity (Brookfield) 40mPa, purity 99.5%) and 61.75g and 3.25g microcrystalline cellulose (25 DEG C, 2%
Aqueous Solution Viscosity (Brookfield) 2mPa, purity 99.8%) mixing, then deaerate 20 points in the case where vacuum degree is 0.10MPa
Clock is filled with nitrogen, and the H that mass percent concentration is 40% is added2SO4Aqueous solution 260mL；
Second step, 40 DEG C keep the temperature 2 hours, centrifuge separation, take precipitating, 30 DEG C of water washings of obtained solid, be centrifugated,
Obtain the solid that water content is 65%；
Third step, the solid that the water content under nitrogen protection obtaining second step is 65%wt, it is mixed to be added 9.5g alkalinity
It closes in object powder (by Na2CO3、K2CO3And (NH4)2CO3Composition；The Na2CO3、 K2CO3And (NH4)2CO3Mass ratio be 85:
14:1.5)；Alkali: carboxymethyl in raw material is 1:2 (molar ratio), heat preservation (35 DEG C of temperature) 1 hour, the solid after being neutralized,
If the solid after gained neutralizes is formulated as the aqueous solution that mass percent concentration is 1%, pH value 8.0；
4th step, third step is neutralized after solid dehydration, drying, crush, obtain the high temperature resistant carboxymethyl cellulose
Plain sodium.
The high temperature resistant sodium carboxymethylcellulose DS=0.90 (Na:0.52, K:0.08), at 25 DEG C, 1% aqueous solution is glutinous
Spending (Brookfield) is 50mPa, purity 99.5%；60 DEG C of stirrings, 1 hour product 1.0%wt Aqueous Solution Viscosity
It (Brookfield) is 32mPa；In proportion raw material CMC, MCC and K (food level sodium carboxymethylcellulose, microcrystalline cellulose and
KCl), at 25 DEG C, 1.0% Aqueous Solution Viscosity (Brookfield) is 30mPa, 60 DEG C of stirrings, 1 hour product 1.0%wt aqueous solution
Viscosity (Brookfield) is 18mPa.
Embodiment 3
A kind of preparation method of high temperature resistant sodium carboxymethylcellulose, includes the following steps:
The first step, by food level sodium carboxymethylcellulose (DS=1.0,1%wt Aqueous Solution Viscosity (Brookfield)
370mPa, purity 99.5%) 36.0g, 4.0g microcrystalline cellulose (25 DEG C, 2%wt Aqueous Solution Viscosity (Brookfield)
2mPa, purity 99.8%) mixing, it then deaerates 10 minutes in the case where vacuum degree is 0.05 MPa, is filled with argon gas, quality hundred is added
Dividing specific concentration is 15% H2SO4Aqueous solution 300mL；
Second step, 10 DEG C keep the temperature 4 hours, centrifuge separation, take precipitating, 10 DEG C of water washings of obtained solid, be centrifugated,
Obtain the solid that water content is 60%；
Third step, under protection of argon gas, the water content that second step is obtained are the solid of 60%wt, and it is mixed that 8.7g alkalinity is added
It closes in object powder (by Na2CO3、K2CO3And (NH4)2CO3Composition；The Na2CO3、K2CO3And (NH4)2CO3Mass ratio be 98:
1.5:0.5)；Alkali: the carboxymethyl in raw material is 1:2 (molar ratio), keeps the temperature 3 hours (30 DEG C of temperature), the solid after being neutralized；
If the solid after gained neutralizes is formulated as the aqueous solution that mass percent concentration is 1%, pH value 8.0；
4th step, third step neutralized after solid dehydration, drying, crushing, obtain high temperature resistant carboxymethyl cellulose
Sodium.
Gained high temperature resistant sodium carboxymethylcellulose DS=0.95 (Na:0.98, K:0.01), 1% Aqueous Solution Viscosity
It (Brookfield) is 420mPa, purity 99.8%, 60 DEG C of stirrings, 1 hour product 1.0%wt Aqueous Solution Viscosity
It (Brookfield) is 204mPa；The mixture that raw material CMC, MCC in proportion is mixed with KCl physical agitation, at 25 DEG C,
1.0% Aqueous Solution Viscosity (Brookfield) is 150mPa, 60 DEG C of stirrings, 1 hour product 1.0%wt Aqueous Solution Viscosity
It (Brookfield) is 80mPa.
Embodiment 4
A kind of preparation method of high temperature resistant sodium carboxymethylcellulose, includes the following steps:
The first step, by food level sodium carboxymethylcellulose (DS=0.96,1%wt Aqueous Solution Viscosity (Brookfield)
800mPa, purity 98.8%) 38g, 2.0g methylcellulose (MC, 25 DEG C, 2%wt Aqueous Solution Viscosity (Brookfield)
10mPa, purity 99.8%) mixing, it then deaerates 15 minutes in the case where vacuum degree is 0.09MPa, is filled with argon gas, quality hundred is added
Dividing specific concentration is 15% H2SO4Aqueous solution 500mL；
Second step, 20 DEG C keep the temperature 3 hours, centrifuge separation, take precipitating, 20 DEG C of water washings of obtained solid, be centrifugated,
Obtain the solid that water content is 65%；
Third step, the solid that the water content under protection of argon gas obtaining second step is 65%wt, it is mixed to be added 8.4g alkalinity
It closes in object powder (by Na2CO3、K2CO3And (NH4)2CO3Composition；The Na2CO3、 K2CO3And (NH4)2CO3Mass ratio be 90:
9.5:0.5)；Alkali: the carboxymethyl in raw material is 1:2 (molar ratio), keeps the temperature 5 hours (20 DEG C of temperature), consolidating after being neutralized
Body；If the solid after gained neutralizes is formulated as the aqueous solution that mass percent concentration is 1%, pH value 8.0；
Solid after 4th step, third step are neutralized is dehydrated, drying, crushes, and obtains high temperature resistant sodium carboxymethylcellulose.
Gained high temperature resistant sodium carboxymethylcellulose DS=0.90 (Na:0.81, K:0.09), 1% Aqueous Solution Viscosity
It (Brookfield) is 950mPa, purity 99.8%, 60 DEG C of stirrings, 1 hour product 1.0%wt Aqueous Solution Viscosity
It (Brookfield) is 384mPa；The mixture of raw material CMC, MC and KCl physical agitation in proportion, at 25 DEG C, 1.0% is water-soluble
Liquid viscosity (Brookfield) be 650mPa, 60 DEG C stirring 1 hour product 1.0%wt Aqueous Solution Viscosity (Brookfield) be
292mPa。
Embodiment 5
A kind of preparation method of high temperature resistant sodium carboxymethylcellulose, includes the following steps:
The first step, by food level sodium carboxymethylcellulose, (DS=0.94,1%wt Aqueous Solution Viscosity (Brookfield) is
800mPa, purity 98.8%) 36.0g, 4.0g hydroxypropyl grade methylcellulose (25 DEG C, 2%wt Aqueous Solution Viscosity
(Brookfield) it is 160mPa, purity 99.8%) mixing, it then deaerates 15 minutes, is filled in the case where vacuum degree is 0.09MPa
15% H is added in argon gas2SO4Aqueous solution 500mL；
Second step, 20 DEG C keep the temperature 3 hours, centrifuge separation, take precipitating, 20 DEG C of water washings of obtained solid, be centrifugated,
Obtain the solid that water content is 65%；
Third step, under protection of argon gas, the water content that second step is obtained are the solid of 65%wt, and it is mixed that 8.4g alkalinity is added
It closes in object powder (by Na2CO3、K2CO3And (NH4)2CO3Composition；The Na2CO3、K2CO3And (NH4)2CO3Mass ratio be 90:
9.5:0.5)；Alkali: carboxymethyl in raw material is 1:2 (molar ratio), keeps the temperature 5 hours (20 DEG C of temperature), the solid after being neutralized,
If the solid after gained neutralizes is formulated as the aqueous solution that mass percent concentration is 1%, pH value 8.0；
4th step, third step is neutralized after solid dehydration, drying, crush, obtain high temperature resistant carboxymethyl cellulose
Sodium.
Gained high temperature resistant sodium carboxymethylcellulose DS=0.90 (Na:0.81, K:0.09), 1.0% Aqueous Solution Viscosity
It (Brookfield) is 950mPa, purity 99.8%, 60 DEG C of stirrings, 1 hour product 1.0%wt Aqueous Solution Viscosity
It (Brookfield) is 416mPa；The mixture of raw material CMC, MCC and KCl physical agitation in proportion is at 25 DEG C, 1.0% water
Solution viscosity (Brookfield) be 650mPa, 60 DEG C stirring 1 hour product 1.0%wt Aqueous Solution Viscosity (Brookfield) be
166mPa。
Above embodiments are only preferrred embodiment of the present invention, for explaining only the invention, are not intended to limit the present invention, this
Field technical staff should belong to guarantor of the invention without departing from change made under spirit of the invention, replacement, modification etc.
Protect range.
Claims (10)
1. a kind of preparation method of high temperature resistant sodium carboxymethylcellulose, which comprises the steps of:
(1) sodium carboxymethylcellulose is mixed with cellulose base foodstuff glue, obtains mixed raw material, is then de-gassed, with
Sulfuric acid solution mixing, isothermal holding, filtering take filter residue；
(2) step (1) described filter residue, the solid after being washed is washed with water；
(3) under an inert atmosphere, the solid after step (2) described washing is added in alkaline mixed-powder, is neutralized,
Solid after being neutralized；
(4) solid after neutralization is dehydrated, drying, crushing obtains the high temperature resistant sodium carboxymethylcellulose.
2. preparation method according to claim 1, which is characterized in that step (1) the cellulose base foodstuff glue is crystallite
One or more of cellulose, methylcellulose and hydroxypropyl grade methylcellulose；The sodium carboxymethylcellulose and cellulose base
The mass ratio of foodstuff glue is 86-99.5:0.5-14.
3. preparation method according to claim 1, which is characterized in that step (1) described degassing process is to be in vacuum degree
It deaerates 5-20 minutes under 0.05-0.10 MPa, is then charged with inert gas；The inert gas is nitrogen, helium or argon gas.
4. preparation method according to claim 1, which is characterized in that the mass percent of step (1) described sulfuric acid solution
Concentration is 10wt% -40wt%；The sulfuric acid solution and the volume mass of mixed raw material ratio are 4-16:1 L/kg.
5. preparation method according to claim 1, which is characterized in that the temperature of step (1) described isothermal holding is 10-40
Degree Celsius, the time of isothermal holding is 2-10 hours.
6. preparation method according to claim 1, which is characterized in that the temperature of step (2) described water is 0-30 degrees Celsius；
The water content of solid after the washing is 55-65%.
7. preparation method according to claim 1, which is characterized in that step (3) inert atmosphere be nitrogen, helium or
Argon atmosphere；The temperature of the neutralisation treatment is 25-35 degrees Celsius, and the time of neutralisation treatment is 1-6 hours.
8. preparation method according to claim 1, which is characterized in that step (3) the alkaline mixed-powder, by weight
Number meter, comprising:
Na2CO385-98 parts；
K2CO31.5-14 part；
(NH4)2CO30.5-1.5 parts.
9. preparation method according to claim 1, which is characterized in that the solid after step (3) described neutralization, if being formulated as
The aqueous solution that mass percent concentration is 1%, pH value 7.5-8.0.
10. a kind of high temperature resistant sodium carboxymethylcellulose as made from claim 1-9 described in any item preparation methods.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB986999A (en) * | 1963-08-21 | 1965-03-24 | Pakistan Council Of Scient And | A process for the production of sodium carboxymethylcellulose from jute and oil-in-water emulsions prepared therefrom |
| US4521594A (en) * | 1983-05-20 | 1985-06-04 | Daicel Chemical Industries, Ltd. | Process for producing sodium carboxymethylcellulose |
| US4525585A (en) * | 1982-10-04 | 1985-06-25 | Daicel Chemical Industries, Ltd. | Sodium carboxymethylcellulose |
| CN101967231A (en) * | 2010-09-30 | 2011-02-09 | 华南理工大学 | Production method of sodium carboxymethyl cellulose with low sodium content |
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2019
- 2019-06-11 CN CN201910503166.8A patent/CN110214932B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB986999A (en) * | 1963-08-21 | 1965-03-24 | Pakistan Council Of Scient And | A process for the production of sodium carboxymethylcellulose from jute and oil-in-water emulsions prepared therefrom |
| US4525585A (en) * | 1982-10-04 | 1985-06-25 | Daicel Chemical Industries, Ltd. | Sodium carboxymethylcellulose |
| US4521594A (en) * | 1983-05-20 | 1985-06-04 | Daicel Chemical Industries, Ltd. | Process for producing sodium carboxymethylcellulose |
| CN101967231A (en) * | 2010-09-30 | 2011-02-09 | 华南理工大学 | Production method of sodium carboxymethyl cellulose with low sodium content |
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