CN104045719A - Method of preparing carboxymethylcellulose by use of manioc waste - Google Patents

Method of preparing carboxymethylcellulose by use of manioc waste Download PDF

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Publication number
CN104045719A
CN104045719A CN201410319566.0A CN201410319566A CN104045719A CN 104045719 A CN104045719 A CN 104045719A CN 201410319566 A CN201410319566 A CN 201410319566A CN 104045719 A CN104045719 A CN 104045719A
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China
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manioc waste
carboxymethyl cellulose
deionized water
sodium hydroxide
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CN201410319566.0A
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Inventor
温国华
杨永启
冯凯
刘广华
郭玉婷
王晨雪
马贺成
莫国莉
陈超
柳青
赵红霞
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Inner Mongolia University
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Inner Mongolia University
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Priority to CN201410319566.0A priority Critical patent/CN104045719A/en
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Abstract

The invention discloses a method of preparing carboxymethylcellulose by use of manioc waste. The method mainly comprises the following craft processes: firstly, continuously stirring 10g of dried manioc waste so as to enable the dried manioc waste to be dispersed to 50g of deionized water; then, adding 0.823-2.47g of sodium hydroxide and soaking for 6 hours at a normal temperature; then, alkalizing for 1.5 hours under a water bath condition of 30 DEG C; heating to 75 DEG C and then adding 2.40-3.595g of sodium chloroacetate; reacting for 1 hour, taking out and drying; smashing and grinding, and then repeating the steps above; repeating the reaction for three times to obtain the carboxymethylcellulose with the degree of substitution within 0.20-1.19.

Description

A kind of method of preparing carboxymethyl cellulose with manioc waste
Technical field
The present invention relates to anti-soil for being applied to detergents and cosmetic articles for washing deposition agent again, the dyeing and printing auxiliary of textile industry, the sizing agent of paper industry, the preparation method of the mud drilling agent of the tackiness agent of feed and ceramic industry and oilfield exploitation and the carboxymethyl cellulose of water retaining, refers to that take manioc waste, sodium chloroacetate prepares the method for carboxymethyl cellulose as main raw material especially.
Background technology
Carboxymethyl cellulose is a kind of water-soluble cellulose ether, and what have practical value is its sodium salt.So generally speaking carboxymethyl cellulose just refers to Xylo-Mucine.The raw material of preparing carboxymethyl cellulose is generally cotton or linters.Because this cost of material is higher, make the high expensive of carboxymethyl cellulose product.
Manioc waste be exactly a kind of main component of producing after being processed into starch or alcohol of cassava be the by product of water, cell debris, starch, Mierocrystalline cellulose and a small amount of protein, usually used as a kind of roughage feeding animals.It is numerous that fresh potato slag carries bacterial classification, is difficult for storing, transporting, and putrid and deteriorated rear generation stench, causes environmental pollution; If dry high cost, increase business burden, usually used as feed or as waste residue, bury processing, as feed animal, do not like to eat, bury the pollution that can cause soil and groundwater, utilize degree lower simultaneously.In potato slag, contain a large amount of Mierocrystalline celluloses, there is very high value of exploiting and utilizing.
It is raw material that this law adopts the waste manioc waste producing in tapioca (flour) production process, manioc waste is made after simple alkaline purification to alkalization Mierocrystalline cellulose, then gradation is at a lower temperature reacted with sodium chloroacetate, final oven dry makes carboxymethyl cellulose product, present method can utilization of waste material alleviate environmental pressure, can significantly reduce costs again, there is good practicality and marketing.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of method of preparing carboxymethyl cellulose with manioc waste, this preparation method take manioc waste, sodium hydroxide, sodium chloroacetate to prepare carboxymethyl cellulose as main raw material, through rational proportion, by certain technological process, make carboxymethyl cellulose.
Technical problem of the present invention is solved by following scheme: a kind of method of preparing carboxymethyl cellulose with manioc waste, it is characterized in that: first the dry manioc waste of 10g is distributed in 50g deionized water under constantly stirring, then add under 0.823g-2.47g sodium hydroxide normal temperature, soak 8 hours, again 35 ℃ of alkalization 1 hour, after being warmed up to 70 ℃, add 2.40g sodium chloroacetate, reaction 2h after at 120 ℃ of dry 48h, after pulverizing and grinding, again repeat above-mentioned steps, repeatedly react three times, can obtain the carboxymethyl cellulose product of substitution value between 0.20-1.19.
Advantage of the present invention is: 1, effectively realize turning waste into wealth of manioc waste, solve manioc waste contaminate environment in industrial production and the problem that cannot rationally process.2, this product be take manioc waste as raw material, because manioc waste contains a large amount of Mierocrystalline celluloses, thereby greatly reduces raw materials cost.3, the raw material of producing this product is manioc waste, and manioc waste derives from cassava, cassava is the very large agricultural-food of province output such as south China Guangxi, Guangdong, Hainan, and the promotion conference of this product is expanded out a new road to the deep processing of south China area agricultural-food, and peasant is increased income.4, the method cost is low and simple to operate, has greatly simplified preparation technology.5, in technological process, by gradation after being ground to small particle size, add sodium hydroxide and sodium chloroacetate, can greatly increase reaction specific surface, improve etherification reaction speed and etherificate degree.
Proportioning raw materials in the present invention and preparation technology compare from the technique of other products all have different significantly, specific as follows: the proportioning raw materials of (1) reactant is the mass ratio of manioc waste, sodium hydroxide, sodium chloroacetate.Proportioning raw materials is one of important factor affecting substituted in reaction degree.(2) preparation process minute secondary response after mechanical disintegration is ground to small particle size prepare carboxymethyl cellulose more traditional once add reaction contact gear ratio surface much bigger and significantly improve substitution value (3) temperature of reaction and the reaction times all first soaks compared with good a lot (4) this reaction preparation technologies of traditional method the etherificate that then heats up that alkalizes again, then drying and crushing reaction repeated three times again, simple to operate, instrument is cheap and easy to get.
Accompanying drawing explanation: Fig. 1. a kind of process flow sheet of preparing carboxymethyl cellulose with manioc waste.
Embodiment:
Embodiment 1: measure 50.0ml deionized water and join in reaction vessel, weigh 10g manioc waste, under the condition constantly stirring, add manioc waste.Take 0.823g dissolution of sodium hydroxide in 5ml deionized water, until heat release completely and sodium hydroxide joined after dissolving completely and in reaction vessel, soaked 6h, then under constantly stirring, be warmed up to 30 ℃ of alkalization 1.5h, accurately take 2.40g sodium chloroacetate dissolved in 10ml deionized water, after being warmed up to 75 ℃, under agitation slowly add above-mentioned solution etherificate 1h, after being dried, being crushed to 80 orders, repeat above-mentioned steps three times, obtain substitution value and be 0.20 carboxymethyl cellulose product;
Embodiment 2: measure 50.0ml deionized water and join in reaction vessel, weigh 10g manioc waste, under the condition constantly stirring, add manioc waste.Take 1.00g dissolution of sodium hydroxide in 5ml deionized water, until heat release completely and sodium hydroxide joined after dissolving completely and in reaction vessel, soaked 6h, then under constantly stirring, be warmed up to 30 ℃ of alkalization 1.5h, accurately take 3.595g sodium chloroacetate dissolved in 10ml deionized water, after being warmed up to 75 ℃, under agitation slowly add above-mentioned solution etherificate 1h, after being dried, being crushed to 80 orders, repeat above-mentioned steps three times, obtain substitution value and be 0.29 carboxymethyl cellulose product;
Embodiment 3: measure 50.0ml deionized water and join in reaction vessel, weigh 10g potato residues, under the condition constantly stirring, add potato residues.Take 1.235g dissolution of sodium hydroxide in 5ml deionized water, until heat release completely and sodium hydroxide joined after dissolving completely and in reaction vessel, soaked 6h, then under constantly stirring, be warmed up to 30 ℃ of alkalization 1.5h, accurately take 2.40g sodium chloroacetate dissolved in 10ml deionized water, after being warmed up to 75 ℃, under agitation slowly add above-mentioned solution etherificate 1h, after being dried, being crushed to 80 orders, repeat above-mentioned steps three times, obtain substitution value and be 0.38 carboxymethyl cellulose product;
Embodiment 4: measure 50.0ml deionized water and join in reaction vessel, weigh 10g potato residues, under the condition constantly stirring, add potato residues.Take 1.65g dissolution of sodium hydroxide in 5ml deionized water, until heat release completely and sodium hydroxide joined after dissolving completely and in reaction vessel, soaked 6h, then under constantly stirring, be warmed up to 30 ℃ of alkalization 1.5h, accurately take 2.40g sodium chloroacetate dissolved in 10ml deionized water, after being warmed up to 75 ℃, under agitation slowly add above-mentioned solution etherificate 1h, after being dried, being crushed to 80 orders, repeat above-mentioned steps three times, obtain substitution value and be 0.58 carboxymethyl cellulose product;
Embodiment 5: measure 50.0ml deionized water and join in reaction vessel, weigh 10g potato residues, under the condition constantly stirring, add potato residues.Take 1.853g dissolution of sodium hydroxide in 5ml deionized water, until heat release completely and sodium hydroxide joined after dissolving completely and in reaction vessel, soaked 6h, then under constantly stirring, be warmed up to 30 ℃ of alkalization 1.5h, accurately take 3.595g sodium chloroacetate dissolved in 10ml deionized water, after being warmed up to 75 ℃, under agitation slowly add above-mentioned solution etherificate 1h, after being dried, being crushed to 80 orders, repeat above-mentioned steps three times, obtain substitution value and be 0.85 carboxymethyl cellulose product;
Embodiment 6: measure 50.0ml deionized water and join in reaction vessel, weigh 10g potato residues, under the condition constantly stirring, add potato residues.Take 2.47g dissolution of sodium hydroxide in 5ml deionized water, until heat release completely and sodium hydroxide joined after dissolving completely and in reaction vessel, soaked 6h, then under constantly stirring, be warmed up to 30 ℃ of alkalization 1.5h, accurately take 3.595g sodium chloroacetate dissolved in 10ml deionized water, after being warmed up to 75 ℃, under agitation slowly add above-mentioned solution etherificate 1h, after being dried, being crushed to 80 orders, repeat above-mentioned steps three times, obtain substitution value and be 1.19 carboxymethyl cellulose.

Claims (3)

1. a method of preparing carboxymethyl cellulose with manioc waste is characterized in that: first dry manioc waste 10g is distributed to and holds 50g deionized water in reaction vessel under constantly stirring, then add 0.823g-2.47g sodium hydroxide carry out soak at room temperature 6 hours, again 30 ℃ alkalization 1.5 hours, after being warmed up to 75 ℃, add 2.40g-3.595g sodium chloroacetate, after reaction 1h, take out dry, after pulverizing and grinding, again repeat above-mentioned steps, repeatedly react three times, get final product to obtain the carboxymethyl cellulose product of substitution value between 0.20-1.19.
2. this technique preparation cost is cheap, and utilization of waste material effectively solves the problem that manioc waste causes environment, and greatly widens the deep processing of cassava, for peasant increases income.
3. this technical process compares with the traditional preparation method of industry that there were significant differences, and technique is simple, is beneficial to the marketization and promotes.
CN201410319566.0A 2014-07-07 2014-07-07 Method of preparing carboxymethylcellulose by use of manioc waste Withdrawn CN104045719A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104761648A (en) * 2015-04-15 2015-07-08 桂林理工大学 Method for preparing nanocellulose at low energy consumption
CN105419752A (en) * 2015-12-01 2016-03-23 中国地质大学(北京) Slurry process for preparing filtrate reducer for water-based drilling fluid by utilizing anaerobic fermentation biogas residues
CN105482787A (en) * 2015-12-01 2016-04-13 中国地质大学(北京) Kneading method for preparing water-based drilling fluid filtrate reducer by using anaerobic fermentation biogas residues
CN108470912A (en) * 2018-04-12 2018-08-31 厦门大学 A kind of preparation method of negative electrode of lithium ion battery using adhesive
CN109024035A (en) * 2018-06-28 2018-12-18 广西驰胜农业科技有限公司 A method of extracting cellulose from manioc waste
CN110079327A (en) * 2019-05-30 2019-08-02 北京理工大学 The preparation method and application of stalk sodium water conservation and conditioning materials

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104761648A (en) * 2015-04-15 2015-07-08 桂林理工大学 Method for preparing nanocellulose at low energy consumption
CN105419752A (en) * 2015-12-01 2016-03-23 中国地质大学(北京) Slurry process for preparing filtrate reducer for water-based drilling fluid by utilizing anaerobic fermentation biogas residues
CN105482787A (en) * 2015-12-01 2016-04-13 中国地质大学(北京) Kneading method for preparing water-based drilling fluid filtrate reducer by using anaerobic fermentation biogas residues
CN105419752B (en) * 2015-12-01 2018-04-03 中国地质大学(北京) A kind of slurry process method that water-base drilling fluid fluid loss additive is prepared using anaerobic fermentation biogas residue
CN105482787B (en) * 2015-12-01 2018-04-03 中国地质大学(北京) A kind of kneading process method that water-base drilling fluid fluid loss additive is prepared using anaerobic fermentation biogas residue
CN108470912A (en) * 2018-04-12 2018-08-31 厦门大学 A kind of preparation method of negative electrode of lithium ion battery using adhesive
CN109024035A (en) * 2018-06-28 2018-12-18 广西驰胜农业科技有限公司 A method of extracting cellulose from manioc waste
CN110079327A (en) * 2019-05-30 2019-08-02 北京理工大学 The preparation method and application of stalk sodium water conservation and conditioning materials

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Application publication date: 20140917