CN102558366A - Preparation method of ammonium carboxymethylcellulose - Google Patents

Preparation method of ammonium carboxymethylcellulose Download PDF

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Publication number
CN102558366A
CN102558366A CN2011104576505A CN201110457650A CN102558366A CN 102558366 A CN102558366 A CN 102558366A CN 2011104576505 A CN2011104576505 A CN 2011104576505A CN 201110457650 A CN201110457650 A CN 201110457650A CN 102558366 A CN102558366 A CN 102558366A
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reaction
cmc
temperature
ammonium
certain amount
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CN102558366B (en
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陈洋溢
张长青
陈静
郭鸿雁
李友琦
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Chongqing Lihong Fine Chemicals Co Ltd
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Chongqing Lihong Fine Chemicals Co Ltd
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Abstract

The invention provides a preparation method of ammonium carboxymethylcellulose, which includes first evenly mixing sodium carboxymethylcellulose powder and dilute sulphuric acid solution in stirring mode, placing the mixture statically for a time, conducting acidification reaction, conducting washing and centrifuging, adding hartshorn to conduct ammonium compounding, finally conducting washing, centrifuging, drying and crushing to obtain a ammonium carboxymethylcellulose product. The whole production process is simple in process, short in reaction period, less in equipment investment and low in raw material consumption.

Description

A kind of preparation method of carboxymethyl cellulose ammonium
Technical field
The present invention relates to a kind of carboxymethyl cellulose ammonium (CMC-NH 4) the preparation method, belong to natural macromolecular material chemical modification field.
Background technology
The coal in China consumption is big, and the environmental pollution that causes thus is particularly serious, wherein flue dust, SO 2And NO xBe principal pollutant.NOx is the main pollutent of thermal power generation discharging, is one of main source of acid rain, or the precursor substance of photo-chemical smog.To form bigger harm to HUMAN HEALTH and ecotope simultaneously.In present various denitration technologies, selective-catalytic-reduction denitrified (SCR) uses maximum, most effective, and its nitric efficiency is 80～90%, even can be up to 95%, and is one of proven technique, and its processing unit is compact, and is reliable.The key of SCR is high performance catalyzer, is matrix with the SCR catalyst powder generally, with shaping assistant etc. through mix, process such as kneading, extrusion molding, drying, roasting obtains.In order to obtain the character homogeneous, the plasticity lotion of better physical strength and pore structure is arranged, need to add tackiness agent, extrusion aid, pore-forming material, spun glass and lubricant etc.Wherein, carboxymethyl cellulose ammonium (CMC-NH 4) be a kind of tackiness agent commonly used, it is good to have cohesiveness, residual few characteristics after the roasting, the domestic CMC-NH that is used for the denitration industry at present 4Main dependence on import generally adopts the ion exchange column method to produce, and cost is higher, and domestic rarely seen production report.The present invention is raw material with CMC-Na, successfully prepares after acidified reaction and the ammonium reaction and satisfies the CMC-NH that denitrating catalyst uses 4Product, and technology is simple, and reaction time is short, and facility investment is few, and raw material consumption is low.
Summary of the invention
It is good that the object of the invention adopts lower-cost chemical synthesis to prepare a kind of solvability, has viscosity performance preferably, and the ash content residual volume after the calcining is few, satisfies the CMC-NH that denitrating catalyst uses 4
Technical scheme of the present invention is following:
A kind of CMC-NH 4The preparation method, it is characterized in that may further comprise the steps:
A, Xylo-Mucine (CMC-Na) and a certain amount of sulphuric acid soln are mixed, carry out acidification reaction;
After b, acidification reaction finish, a certain amount of water is added in the product agitator treating, spinning.
C, product that obtains among the step b and certain amount of ammonia water ethanolic soln are mixed, carry out the ammonium reaction;
D, with the material spinning after the ammoniumization;
E, with the oven dry of the product that obtains in the steps d, pulverize.
The mass percent concentration of said sulphuric acid soln is 10～40%, is reaction medium with the aqueous ethanolic solution among the step c, and the mass percentage concentration of aqueous ethanolic solution is 70～95%, and the mass percentage concentration of ammoniacal liquor is 10～25%.
Mass ratio 6.5～9.0:1 of sulphuric acid soln and CMC;
Mass ratio 2.0～4.0:1 of ethanolic soln and CMC;
Mass ratio 0.5～3.0:1 of ammoniacal liquor and CMC.
Wherein, the acidification reaction time is 100～200min among the step a, and temperature of reaction is a normal temperature.
Among the step c, the ammonium reaction times is 150～250min, and temperature of reaction is a normal temperature.
Among the step e, bake out temperature is 60～80 ℃, prevents the too high volatilization that causes ammonia of temperature.
The inventive method production process technology is simple, and reaction time is short, and facility investment is few, and raw material consumption is low, and the carboxymethyl cellulose ammonium that adopts this method to produce has viscosity performance preferably, and the ash content residual volume after the calcining seldom simultaneously.
Description of drawings
Fig. 1 is a Production Flow Chart block diagram of the present invention.
Embodiment
Below in conjunction with Fig. 1 and embodiment the present invention is further described.
Embodiment 1:
With a certain amount of Xylo-Mucine powder (2%NDJ-79 viscosity 850, substitution value 0.62), concentration 10% aqueous sulfuric acid of 6.5 times of quality behind the stirring 60min, leaves standstill acidifying 40min again; Then a certain amount of water is added in the product agitator treating, spinning; The concentration that centrifugal back adds 0.5 times of quality is 10% ammonia soln; The concentration that adds 2.0 times of quality simultaneously is 70% ethanolic soln; Standing and reacting 150min behind the stirring and evenly mixing, and then spinning, and in baking oven, dry 120min; Bake out temperature is 60～80 ℃, obtains refining CMC-NH after the pulverizing 4Finished product, 1% solution viscosity that Brookfield type viscometer is measured is 92, ash oontent 0.20%.
Embodiment 2:
With a certain amount of Xylo-Mucine powder (2%NDJ-79 viscosity 850, substitution value 0.62), concentration 20% aqueous sulfuric acid of 7.5 times of quality behind the stirring 60min, leaves standstill acidifying 90min again; A certain amount of water is added in the product agitator treating, spinning; The concentration that centrifugal back adds 1.0 times of quality is 15% ammonia soln; The concentration that adds 4.0 times of quality simultaneously is 80% ethanolic soln; Standing and reacting 180min behind the stirring and evenly mixing, and then spinning, and in baking oven, dry 120min; Bake out temperature is 60～80 ℃, obtains refining CMC-NH after the pulverizing 4Finished product, 1% solution viscosity that Brookfield type viscometer is measured is 97, ash oontent 0.15%.
Embodiment 3:
With a certain amount of Xylo-Mucine powder (2%NDJ-79 viscosity 850, substitution value 0.62), concentration 20% aqueous sulfuric acid of 8.0 times of quality behind the stirring 60min, leaves standstill acidifying 120min again; Remove supernatant liquid then, a certain amount of water is added in the product agitator treating, spinning; The concentration that centrifugal back adds 1.5 times of quality is 20% ammonia soln; The concentration that adds 3.0 times of quality simultaneously is 90% ethanolic soln; Standing and reacting 210min behind the stirring and evenly mixing, and then spinning, and in baking oven, dry 120min; Bake out temperature is 60～80 ℃, obtains refining CMC-NH after the pulverizing 4Finished product, 1% solution viscosity that Brookfield type viscometer is measured is 105, ash oontent 0.08%.
Embodiment 4:
With a certain amount of Xylo-Mucine powder (2%NDJ-79 viscosity 510, substitution value 0.85), concentration 30% aqueous sulfuric acid of 9.0 times of quality behind the stirring 60min, leaves standstill acidifying 120min again; A certain amount of water is added in the product agitator treating, spinning; The concentration that centrifugal back adds 2.5 times of quality is 25% ammonia soln; The concentration that adds 3.0 times of quality simultaneously is 90% ethanolic soln; Standing and reacting 240min behind the stirring and evenly mixing, and then spinning, and in baking oven, dry 120min; Bake out temperature is 60～80 ℃, obtains refining CMC-NH after the pulverizing 4Finished product, 1% solution viscosity that Brookfield type viscometer is measured is 50, ash oontent 0.08%.
Embodiment 5:
With a certain amount of Xylo-Mucine powder (2%NDJ-79 viscosity 1350, substitution value 0.72), concentration 40% aqueous sulfuric acid of 8.0 times of quality behind the stirring 60min, leaves standstill acidifying 140min again; A certain amount of water is added in the product agitator treating, spinning; The concentration that centrifugal back adds 3.0 times of quality is 25% ammonia soln; The concentration that adds 3.0 times of quality simultaneously is 95% ethanolic soln; Standing and reacting 250min behind the stirring and evenly mixing, and then spinning, and in baking oven, dry 120min; Bake out temperature is 60～80 ℃, obtains refining CMC-NH after the pulverizing 4Finished product, 1% solution viscosity that Brookfield type viscometer is measured is 95, ash oontent 0.07%.
Term:
viscosity: 1% aqueous solution, 1% aqueous solution Type B viscosity detects under 25 ℃ of conditions.
ash content: ash oontent.

Claims (4)

1. the preparation method of a carboxymethyl cellulose ammonium is characterized in that may further comprise the steps:
A, Xylo-Mucine (CMC-Na) and a certain amount of sulphuric acid soln are mixed, carry out acidification reaction;
After b, acidification reaction finish, a certain amount of water is added in the product agitator treating, spinning;
C, product that obtains among the step b and certain amount of ammonia water ethanolic soln are mixed, carry out the ammonium reaction;
D, with the material spinning after the ammoniumization;
E, with the oven dry of the product that obtains in the steps d, pulverize;
The mass percent concentration of said sulphuric acid soln is 10～40%, is reaction medium with the aqueous ethanolic solution among the step c, and the mass percentage concentration of aqueous ethanolic solution is 70～95%, and the mass percentage concentration of ammoniacal liquor is 10～25%;
Mass ratio 6.5～9.0:1 of sulphuric acid soln and CMC;
Mass ratio 2.0～4.0:1 of ethanolic soln and CMC;
Mass ratio 0.5～3.0:1 of ammoniacal liquor and CMC.
2. the method for preparing carboxymethyl cellulose ammonium according to claim 1 is characterized in that: the acidification reaction time is 100～200min among the step a, and temperature of reaction is a normal temperature.
3. the method for preparing carboxymethyl cellulose ammonium according to claim 1 is characterized in that: among the step c, the reaction times is 150～250min, and temperature of reaction is a normal temperature.
4. the method for preparing carboxymethyl cellulose ammonium according to claim 1 is characterized in that: among the step e, bake out temperature is 60～80 ℃, prevents the too high volatilization that causes ammonia of temperature.
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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103242454A (en) * 2013-05-13 2013-08-14 宜兴市通达化学有限公司 Method for preparing high-substitution degree ammonium carboxymethyl cellulose by means of mixed strong acid
CN106336462A (en) * 2016-10-13 2017-01-18 重庆力宏精细化工有限公司 Method for preparing carboxymethyl cellulose
CN106496336A (en) * 2016-11-25 2017-03-15 泸州北方化学工业有限公司 The method that nitrate method prepares carboxymethyl cellulose ammonium
CN108715617A (en) * 2018-04-25 2018-10-30 山东滕新材料股份有限公司 Native cellulose prepares carboxymethyl cellulose ammonium
CN109609036A (en) * 2018-12-06 2019-04-12 武汉科丝力纤维制造有限公司 A kind of environment-friendly modified foamed ceramics adhesive and its preparation process
CN109627349A (en) * 2018-11-30 2019-04-16 泸州北方纤维素有限公司 The ammonium chemical industry skill of carboxymethyl cellulose ammonium
CN110467682A (en) * 2019-09-24 2019-11-19 北京理工大学 A kind of cellulose derivative and its preparation method and application
CN112321730A (en) * 2020-11-10 2021-02-05 重庆纤磊新材料科技有限公司 Preparation method of high-viscosity carboxymethyl cellulose ammonium
CN114335541A (en) * 2021-12-29 2022-04-12 蜂巢能源科技股份有限公司 Positive electrode slurry and preparation method and application thereof
CN115260943A (en) * 2022-07-14 2022-11-01 向能新型材料科技(河北)有限公司 Preparation method of carboxymethyl cellulose ammonium aqueous adhesive

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1265922A (en) * 2000-01-27 2000-09-13 华南理工大学 Process for preparing calcium carboxymethyl cellulose
CN102206286A (en) * 2011-05-16 2011-10-05 北京理工大学 Preparation method of lithium carboxymethyl cellulose for lithium battery

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1265922A (en) * 2000-01-27 2000-09-13 华南理工大学 Process for preparing calcium carboxymethyl cellulose
CN102206286A (en) * 2011-05-16 2011-10-05 北京理工大学 Preparation method of lithium carboxymethyl cellulose for lithium battery

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103242454A (en) * 2013-05-13 2013-08-14 宜兴市通达化学有限公司 Method for preparing high-substitution degree ammonium carboxymethyl cellulose by means of mixed strong acid
CN106336462A (en) * 2016-10-13 2017-01-18 重庆力宏精细化工有限公司 Method for preparing carboxymethyl cellulose
CN106496336A (en) * 2016-11-25 2017-03-15 泸州北方化学工业有限公司 The method that nitrate method prepares carboxymethyl cellulose ammonium
CN108715617A (en) * 2018-04-25 2018-10-30 山东滕新材料股份有限公司 Native cellulose prepares carboxymethyl cellulose ammonium
CN109627349A (en) * 2018-11-30 2019-04-16 泸州北方纤维素有限公司 The ammonium chemical industry skill of carboxymethyl cellulose ammonium
CN109609036A (en) * 2018-12-06 2019-04-12 武汉科丝力纤维制造有限公司 A kind of environment-friendly modified foamed ceramics adhesive and its preparation process
CN110467682A (en) * 2019-09-24 2019-11-19 北京理工大学 A kind of cellulose derivative and its preparation method and application
CN112321730A (en) * 2020-11-10 2021-02-05 重庆纤磊新材料科技有限公司 Preparation method of high-viscosity carboxymethyl cellulose ammonium
CN114335541A (en) * 2021-12-29 2022-04-12 蜂巢能源科技股份有限公司 Positive electrode slurry and preparation method and application thereof
CN115260943A (en) * 2022-07-14 2022-11-01 向能新型材料科技(河北)有限公司 Preparation method of carboxymethyl cellulose ammonium aqueous adhesive

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