CN105254769A - Method for preparing technical grade sodium carboxymethyl cellulose - Google Patents
Method for preparing technical grade sodium carboxymethyl cellulose Download PDFInfo
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- CN105254769A CN105254769A CN201510824422.5A CN201510824422A CN105254769A CN 105254769 A CN105254769 A CN 105254769A CN 201510824422 A CN201510824422 A CN 201510824422A CN 105254769 A CN105254769 A CN 105254769A
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Abstract
The invention belongs to the field of chemical engineering, in particular relates to a method for preparing technical grade sodium carboxymethyl cellulose, and aims to solve the technical problem of providing a method for preparing technical grade sodium carboxymethyl cellulose. The method comprises the following steps: a, mixing alcohol and a sodium hydroxide solution so as to obtain a mixed liquid; b, uniformly mixing the mixed liquid and a cellulose raw material for alkalization reaction; c, adding an etherifying agent into the material obtained after alkalization reaction in the step b; d, mixing alcohol with the sodium hydroxide solution so as to obtain another mixed liquid; e, uniformly mixing the mixed liquid obtained in the step d with the material obtained after etherification reaction in the step c for alkalization reaction; f, adding an oxidant and alcohol into the material obtained after alkalization reaction in the step d for refining and viscosity reduction. By adopting the method, the technical grade sodium carboxymethyl cellulose with low velocity can be prepared, the purity can be greater than 75%, and the etherification efficiency can be greater than 70%.
Description
Technical field
The invention belongs to chemical field, be specifically related to a kind of method of technology of preparing level sodium carboxymethylcellulose.
Background technology
The low sticky Xylo-Mucine of technical grade is domestic appearance grade oil Xylo-Mucine product type comparatively early, is applicable to shallow well and deep-well shallow-layer district, so consumption is very big.The landing dehydration effect in drilling fluid, cementing fluid and fracturing liquid of the low sticky Xylo-Mucine of technical grade, thus the effect reaching retaining wall, protect drill bit, prevent mud loss, improve drilling speed.
Prior art generally adopts an alkalization method to prepare Xylo-Mucine, but reaction etherificate efficiency is about 65%, product performance index apparent viscosity, substantially at 80 ~ 90mpa.s, is in the index upper limit, can not meet the demand of existing oil field to Xylo-Mucine.
Summary of the invention
For the problem existing for existing Xylo-Mucine, goal of the invention of the present invention is a kind of method providing technology of preparing level sodium carboxymethylcellulose.The etherificate efficiency of the method is up to 70%, and the viscosity of the Xylo-Mucine prepared is lower than 80mpa.s.
Technical problem to be solved by this invention is to provide a kind of method of technology of preparing level sodium carboxymethylcellulose.The method comprises the following steps:
A, preparation mixed solution: by 225 ~ 270 parts of alcohol and 100 ~ 140 parts of aqueous sodium hydroxide solution mixings, control temperature is 35 ~ 50 DEG C; Add 1.5 ~ 6 parts of hydrogen peroxide more wherein, control temperature is 35 ~ 50 DEG C, obtains mixed solution;
B, alkalization: controlling reaction unit temperature is 25 DEG C ~ 45 DEG C, join the mixed solution of the wood pulp of 50 ~ 70 parts of cp≤40mpa.s or bamboo pulp, step a in reaction unit and carry out quaternization; Reinforced start to alkalization finishing control temperature be 25 ~ 65 DEG C, reinforced terminate to the time after terminating of alkalizing be 70 ~ 110min;
C, etherificate: the etherifying agent of 70 ~ 90 parts is joined in the material of step b reaction end and carry out etherification reaction; Reinforced to start to etherificate finishing control temperature be 40 ~ 65 DEG C, and the reinforced time starting to terminate to etherificate is 35 ~ 65min; Described etherifying agent is concentration 73.0 ~ 75.0% (w/w) Mono Chloro Acetic Acid spirituous solution;
D, again prepare mixed solution: by 80 ~ 120 parts of alcohol and 35 ~ 50 parts of aqueous sodium hydroxide solutions mixings, controlling mixeding liquid temperature is 35 ~ 50 DEG C, obtains mixed solution;
E, alkalization: the mixed solution of steps d is joined in the material of step c reaction end and carry out quaternization; Reinforced to start to alkalization finishing control temperature be 40 ~ 70 DEG C, and the reinforced time starting to terminate to alkalization is 10 ~ 20min; Be warming up to 76 ~ 78 DEG C of constant temperature 25 ~ 35min again; Be cooled to less than 50 DEG C again;
F, refining viscosity reduction: oxygenant, 1750 ~ 2500 parts of alcohol are joined in the material that step e reaction terminates, centrifugal after stirring, dry, pulverize, pack; Described oxygenant is 3 ~ 10 parts of hydrogen peroxide or 1.5 ~ 10 parts of clorox;
Above-mentioned number represents the molar weight of each raw material; If this raw material is solution, number then represents the molar weight of its solute.
Preferably, in the method steps a of above-mentioned technology of preparing level sodium carboxymethylcellulose, the concentration of described alcohol is 90 ~ 95% (v/v); The concentration of described aqueous sodium hydroxide solution is 48.0 ~ 50.0% (w/w).
Preferably, in the method steps a of above-mentioned technology of preparing level sodium carboxymethylcellulose, the massfraction of described hydrogen peroxide is more than 27.5%, described in add hydrogen peroxide be add carrying out 5 ~ 10min before step b.
Preferably, in the method steps b of above-mentioned technology of preparing level sodium carboxymethylcellulose, described reinforced start to the time of reinforced end be 10 ~ 15min.
Preferably, in the method steps c of above-mentioned technology of preparing level sodium carboxymethylcellulose, described etherifying agent with massfraction >=97.5% Mono Chloro Acetic Acid be solute, 90 ~ 95% (v/v) alcohol is that solvent is formulated.
Preferably, in the method steps c of above-mentioned technology of preparing level sodium carboxymethylcellulose, described etherification reaction is: the etherifying agent of 70 ~ 90 parts is joined in 20 ~ 25min step b reaction terminate after material at 40 ~ 50 DEG C, stir 5 ~ 10min, then be warming up to 60 ~ 65 DEG C of constant temperature 15 ~ 20min in 5 ~ 10min.
Preferably, in the method steps d of above-mentioned technology of preparing level sodium carboxymethylcellulose, the concentration of described alcohol is 90 ~ 95% (v/v); The concentration of described aqueous sodium hydroxide solution is 48.0 ~ 50.0% (w/w).
Preferably, in the method steps e of above-mentioned technology of preparing level sodium carboxymethylcellulose, described in be warming up to 76 ~ 78 DEG C for be warming up to 76 ~ 78 DEG C in 15 ~ 20min.
Preferably, in the method steps f of above-mentioned technology of preparing level sodium carboxymethylcellulose, described ethanol concn is 65 ~ 75% (v/v).
Preferably, in the method steps f of above-mentioned technology of preparing level sodium carboxymethylcellulose, described churning time is 5 ~ 30min.
The inventive method can make etherificate efficiency reach more than 70%, improves more than 5% than original method, and the apparent viscosity of the technology level sodium carboxymethylcellulose that the inventive method prepares is lower than 80mps.
Embodiment
A method for technology of preparing level sodium carboxymethylcellulose, comprises the following steps:
A, preparation mixed solution: be 90 ~ 95% (v/v) alcohol and 100 ~ 140 parts of concentration by 225 ~ 270 parts of concentration be the mixing of 48.0 ~ 50.0% (w/w) aqueous sodium hydroxide solution, control temperature is 35 ~ 50 DEG C; Add 1.5 ~ 6 parts of hydrogen peroxide more wherein, control temperature is 35 ~ 50 DEG C, obtains mixed solution;
B, alkalization: controlling reaction unit temperature is 25 DEG C ~ 45 DEG C, joins in reaction unit, joined the wood pulp of 50 ~ 70 parts of cp≤40mpa.s or bamboo pulp in reaction unit by the mixed solution of step a simultaneously and carry out quaternization in 10 ~ 15min; Reinforced start to alkalization finishing control temperature be 25 ~ 65 DEG C, reinforced terminate to the time after terminating of alkalizing be 70 ~ 110min;
C, etherificate: the etherifying agent of 70 ~ 90 parts is joined in 15 ~ 25min step b reaction terminate after material at 40 ~ 50 DEG C, stir 5 ~ 10min, then be warming up to 60 ~ 65 DEG C of constant temperature 10 ~ 20min in 5 ~ 10min; Described etherifying agent with massfraction >=97.5% Mono Chloro Acetic Acid be solute, 90 ~ 95% (v/v) alcohol is that solvent is formulated, the concentration of etherifying agent is 73.0 ~ 75.0% (w/w);
D, again prepare mixed solution: be 90 ~ 95% (v/v) alcohol and 35 ~ 50 parts of concentration by 80 ~ 120 parts of concentration be the mixing of 48.0 ~ 50.0% (w/w) aqueous sodium hydroxide solution, controlling mixeding liquid temperature is 35 ~ 50 DEG C, obtains mixed solution;
E, alkalization: the mixed solution of steps d is joined in the material of step c reaction end and carry out quaternization; Reinforced to start to alkalization finishing control temperature be 40 ~ 70 DEG C, and the reinforced time starting to terminate to alkalization is 10 ~ 20min; In 15 ~ 20min, be warming up to 76 ~ 78 DEG C of constant temperature 25 ~ 35min again, then be cooled to less than 50 DEG C;
F, refining viscosity reduction: be the mixing of 65 ~ 75% (v/v) alcohol by oxygenant and 1750 ~ 2500 parts of concentration, add wherein by the material that step e reaction terminates, centrifugal after stirring 5 ~ 30min, dry, pulverize, pack; Described oxygenant is 3 ~ 10 parts of hydrogen peroxide or 1.5 ~ 10 parts of clorox; Above-mentioned number represents the molar weight of each raw material; If this raw material is solution, number then represents the molar weight of its solute.
In the inventive method, such as: 1) when raw material is solution, as part aqueous sodium hydroxide solution of 100 ~ 140 in step a, expression purity is the molar weight of the sodium hydrate solid of 100% is 100 ~ 140 parts, if the solid sodium hydroxide purity adopted is not 100%, take again after so converting with regard to needs, then join in corresponding water, be mixed with the aqueous sodium hydroxide solution of respective concentration; 2) when raw material is originally as liquid, as 1.5 ~ 10 parts of clorox in step f, represent that the molar weight of pure clorox is 1.5 ~ 10 parts.
Embodiment 1
(1), preparation mixed solution: be that 48.34% (w/w) liquid caustic soda of 93% (v/v) alcohol and 115 parts is mixed to get mixed solution by 250 parts of concentration, and to control mixeding liquid temperature be 40 DEG C ~ 45 DEG C; Before feeding intake, 3.5 parts of hydrogen peroxide add in alkali liquor mixture by 5min, and after mixing, temperature controls at 40 DEG C ~ 45 DEG C;
(2), alkalize: control to mediate built-in temperature 40 DEG C ~ 45 DEG C, in 10 ~ 12min, the Mierocrystalline cellulose wood pulp 63 parts of cp=26mpa.s is added in kneader, prepared for step (1) mixed solution is joined in kneader by shower simultaneously, mixed solution joining day 12 ~ 15min, the quaternization time (not comprising charging time) is 100min, controls quaternization temperature 40 DEG C ~ 65 DEG C;
(3), etherificate: the material after quaternization adds 74.04% (w/w) Mono Chloro Acetic Acid spirituous solution 75 parts by shower, and the interpolation time is 20min, stirs 5min afterwards; Heated up by 5min again, to 61 ~ 63 DEG C of constant temperature 15min; Etherification reaction temperature is 40 DEG C ~ 63 DEG C;
(4), again prepare mixed solution: 48.34% (w/w) liquid caustic soda of 93% (v/v) alcohol of 100 parts and 40 parts is mixed to get mixed solution, and to control mixeding liquid temperature be 40 DEG C ~ 45 DEG C;
(5), alkalize: in the material after terminating to etherification reaction, add step (4) solution by shower, joining day is 5min, after stirring 5min, be warming up to 76 DEG C ~ 78 DEG C constant temperature 30min by 15min, be cooled to less than 50 DEG C and enter treating process;
(6), refining viscosity reduction process: add 73% (v/v) alcohol 2100 parts in washing kettle, then slowly add 3.5 parts of hydrogen peroxide and stir; After mixing, step (5) material is put into washing kettle, stir 20min and after viscosity reduction, carry out centrifugal dewatering, oven dry, pulverizing, pack to obtain the low sticky Xylo-Mucine of finished product technical grade.
The carrying out adopting GB GB/T5005-2010 to contrast the product performance (see table 2) of the Xylo-Mucine that the product performance (see table 1) of the technology level sodium carboxymethylcellulose that the inventive method prepares and existing method prepare contrasts.
Table 1
Table 2
In summary it can be seen, technology level sodium carboxymethylcellulose viscosity prepared by the inventive method is lower, and etherificate rate reaches more than 70%, thus provides a more efficiently method for the preparation of technology level sodium carboxymethylcellulose.
Claims (10)
1. a method for technology of preparing level sodium carboxymethylcellulose, is characterized in that: comprise the following steps:
A, preparation mixed solution: by 225 ~ 270 parts of alcohol and 100 ~ 140 parts of aqueous sodium hydroxide solution mixings, control temperature is 35 ~ 50 DEG C; Add 1.5 ~ 6 parts of hydrogen peroxide more wherein, control temperature is 35 ~ 50 DEG C, obtains mixed solution;
B, alkalization: controlling reaction unit temperature is 25 DEG C ~ 45 DEG C, join the mixed solution of the wood pulp of 50 ~ 70 parts of cp≤40mpa.s or bamboo pulp, step a in reaction unit and carry out quaternization; Reinforced start to alkalization finishing control temperature be 25 ~ 65 DEG C, reinforced terminate to the time after terminating of alkalizing be 70 ~ 110min;
C, etherificate: the etherifying agent of 70 ~ 90 parts is joined in the material of step b reaction end and carry out etherification reaction; Reinforced to start to etherificate finishing control temperature be 40 ~ 65 DEG C, and the reinforced time starting to terminate to etherificate is 35 ~ 65min; Described etherifying agent is concentration 73.0 ~ 75.0% (w/w) Mono Chloro Acetic Acid spirituous solution;
D, again prepare mixed solution: by 80 ~ 120 parts of alcohol and 35 ~ 50 parts of aqueous sodium hydroxide solutions mixings, controlling mixeding liquid temperature is 35 ~ 50 DEG C, obtains mixed solution;
E, alkalization: the mixed solution of steps d is joined in the material of step c reaction end and carry out quaternization; Reinforced to start to alkalization finishing control temperature be 40 ~ 70 DEG C, and the reinforced time starting to terminate to alkalization is 10 ~ 20min; Be warming up to 76 ~ 78 DEG C of constant temperature 25 ~ 35min again; Be cooled to less than 50 DEG C again;
F, refining viscosity reduction: oxygenant, 1750 ~ 2500 parts of alcohol are joined in the material that step e reaction terminates, centrifugal after stirring, dry, pulverize, pack; Described oxygenant is 3 ~ 10 parts of hydrogen peroxide or 1.5 ~ 10 parts of clorox;
Above-mentioned number represents the molar weight of each raw material; If this raw material is solution, number then represents the molar weight of its solute.
2. the method for technology of preparing level sodium carboxymethylcellulose according to claim 1, is characterized in that: in step a, and the concentration of described alcohol is 90 ~ 95% (v/v); The concentration of described aqueous sodium hydroxide solution is 48.0 ~ 50.0% (w/w).
3. the method for technology of preparing level sodium carboxymethylcellulose according to claim 1, is characterized in that: in step a, and the massfraction of described hydrogen peroxide is more than 27.5%, described in add hydrogen peroxide be add carrying out 5 ~ 10min before step b.
4. the method for technology of preparing level sodium carboxymethylcellulose according to claim 1, is characterized in that: in step b, described reinforced start to the time of reinforced end be 10 ~ 15min.
5. the method for technology of preparing level sodium carboxymethylcellulose according to claim 1, is characterized in that: in step c, described etherifying agent with massfraction >=97.5% Mono Chloro Acetic Acid be solute, 90 ~ 95% (v/v) alcohol is that solvent is formulated.
6. the method for technology of preparing level sodium carboxymethylcellulose according to claim 1, it is characterized in that: in step c, described etherification reaction is: the etherifying agent of 70 ~ 90 parts is joined in 20 ~ 25min step b reaction terminate after material at 40 ~ 50 DEG C, stir 5 ~ 10min, then be warming up to 60 ~ 65 DEG C of constant temperature 15 ~ 20min in 5 ~ 10min.
7. the method for technology of preparing level sodium carboxymethylcellulose according to claim 1, is characterized in that: in steps d, and the concentration of described alcohol is 90 ~ 95% (v/v); The concentration of described aqueous sodium hydroxide solution is 48.0 ~ 50.0% (w/w).
8. the method for technology of preparing level sodium carboxymethylcellulose according to claim 1, is characterized in that: in step e, described in be warming up to 76 ~ 78 DEG C for be warming up to 76 ~ 78 DEG C in 15 ~ 20min.
9. the method for technology of preparing level sodium carboxymethylcellulose according to claim 1, is characterized in that: in step f, and described ethanol concn is 65 ~ 75% (v/v).
10. the method for technology of preparing level sodium carboxymethylcellulose according to claim 1, is characterized in that: in step f, and described churning time is 5 ~ 30min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109679595A (en) * | 2018-12-07 | 2019-04-26 | 泸州北方纤维素有限公司 | The method for reducing the low viscous carboxymethyl cellulose cost of technical grade |
| CN112194731A (en) * | 2020-09-21 | 2021-01-08 | 湖州展望药业有限公司 | Injection-grade low-viscosity sodium carboxymethylcellulose and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101747442A (en) * | 2008-12-19 | 2010-06-23 | 丹尼斯克（张家港）亲水胶体有限公司 | The low-viscose granulation method of technology level sodium carboxymethylcellulose |
| CN102286108A (en) * | 2011-07-12 | 2011-12-21 | 重庆力宏精细化工有限公司 | Method for preparing potassium carboxymethylcellulose |
| CN103554273A (en) * | 2013-10-31 | 2014-02-05 | 泸州北方化学工业有限公司 | Production method of technical-grade sodium carboxymethylcellulose |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101747442A (en) * | 2008-12-19 | 2010-06-23 | 丹尼斯克（张家港）亲水胶体有限公司 | The low-viscose granulation method of technology level sodium carboxymethylcellulose |
| CN102286108A (en) * | 2011-07-12 | 2011-12-21 | 重庆力宏精细化工有限公司 | Method for preparing potassium carboxymethylcellulose |
| CN103554273A (en) * | 2013-10-31 | 2014-02-05 | 泸州北方化学工业有限公司 | Production method of technical-grade sodium carboxymethylcellulose |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109679595A (en) * | 2018-12-07 | 2019-04-26 | 泸州北方纤维素有限公司 | The method for reducing the low viscous carboxymethyl cellulose cost of technical grade |
| CN112194731A (en) * | 2020-09-21 | 2021-01-08 | 湖州展望药业有限公司 | Injection-grade low-viscosity sodium carboxymethylcellulose and preparation method thereof |
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Effective date of registration: 20210702 Address after: 646003 Gaoba Luzhou North cellulose Co., Ltd., Longmatan District, Luzhou City, Sichuan Province Patentee after: LUZHOU BEIFANG CELLULOSE Co.,Ltd. Address before: 646003 Sichuan Luzhou high dam Luzhou North Chemical Industry Co., Ltd. Patentee before: LUZHOU NORTH CHEMICAL INDUSTRY Co.,Ltd. |