CN102587182A - Preparation method of microcrystalline cellulose for toothpaste - Google Patents

Preparation method of microcrystalline cellulose for toothpaste Download PDF

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Publication number
CN102587182A
CN102587182A CN201210024162XA CN201210024162A CN102587182A CN 102587182 A CN102587182 A CN 102587182A CN 201210024162X A CN201210024162X A CN 201210024162XA CN 201210024162 A CN201210024162 A CN 201210024162A CN 102587182 A CN102587182 A CN 102587182A
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China
Prior art keywords
microcrystalline cellulose
toothpaste
open
preparation
minute
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CN201210024162XA
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Chinese (zh)
Inventor
周卫东
朱岩
陈晓雪
徐玉勋
张学全
毕勇
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ANHUI SHANHE PHARMACEUTICAL EXCIPIENTS Co Ltd
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ANHUI SHANHE PHARMACEUTICAL EXCIPIENTS Co Ltd
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Priority to CN201210024162XA priority Critical patent/CN102587182A/en
Publication of CN102587182A publication Critical patent/CN102587182A/en
Pending legal-status Critical Current

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  • Polysaccharides And Polysaccharide Derivatives (AREA)

Abstract

A preparation method of microcrystalline cellulose for toothpaste comprises the following steps: 1), hydrolyzing; 2) bleaching; 3) centrifugally washing; 4) granulating; 5) drying; 6) pulverizing; 7) sieving; and 8) secondarily pulverizing. The preparation method of the microcrystalline cellulose for the toothpaste has the technical effects as follows: in the preparation method, wood fiber with the content of refined cotton and hemicellulose of 30-40 percent in a certain ratio is taken as a raw material, and is hydrolyzed by low-concentration dilute hydrochloric acid, sodium hypochlorite is added for bleaching the wood fiber in the hydrolysis process, the hydrolyzing reaction time is shortened, and the wood fiber is dried and primarily pulverized and then pulverized by an ultramicro pulverizer to prepare the microcrystalline cellulose for the toothpaste. The microcrystalline cellulose is high in water absorption, and high in viscosity and free of layering after dissolution in water; the whiteness is greater than 95; and the average particle size is less than 5 microns.

Description

Toothpaste is used the Preparation of microcrystalline cellulose method
Technical field
The present invention relates to a kind of Preparation of microcrystalline cellulose method, relate in particular to a kind of toothpaste and use the Preparation of microcrystalline cellulose method.
Background technology
The toothpaste thickener uses sodium carboxymethylcellulose usually, but sodium carboxymethylcellulose is used chemical industry materials such as solid sodium hydroxide, monoxone and ethanol in building-up process by cotton fiber, and residual being prone to of chemical industry material produces harmful effect to human body.Therefore the raising and the environment protection requirement of Along with people's consumption idea use the synthetic natural thickener of no chemical industry to become future development trend.
Microcrystalline cellulose, therefore is widely used in food and the medicine, and does not in use receive PH, Influence of Temperature because of nontoxic, nonirritant as the Purely natural vegetality cellulose, is desirable thickener.But at present some drawbacks limit of plain edition microcrystalline cellulose its application aspect the toothpaste thickener, the one, plain edition microcrystalline cellulose water absorption rate is low, viscosity causes thickening effect poor inadequately; The 2nd, whiteness is not enough, is unfavorable for the appearance looks elegant of toothpaste; The 3rd, particle diameter is fine and smooth inadequately, and toothpaste has grittiness when using.
Summary of the invention
The present invention is directed to that the thickening property that the plain edition microcrystalline cellulose exists when using as the toothpaste thickener is not enough, whiteness reaches the fine and smooth inadequately defective of particle diameter inadequately and prior preparation method is improved, aim to provide a kind of toothpaste and use the Preparation of microcrystalline cellulose method.
The present invention realizes that like this method step is:
1) hydrolysis: put the 1300Kg drinking water in agitated reactor, open the technical hydrochloric acid measuring tank, it is 0.15-0.20mol/L that the input technical hydrochloric acid makes acidity; Open and be steam heated to 60-80 ℃, close admission valve, start stirring; With the 50kg purified cotton that is torn into flakelet and 50kg hemicellulose level is that 30 ~ 40% xylon drops in the agitated reactor, and the purified cotton average degree of polymerization is 1600-2000, and whiteness is greater than 85; The xylon whiteness is greater than 85; Feed intake finish after, open steam valve and be warmed up to 100 ℃, under this temperature, be hydrolyzed the reaction 8-10 minute;
2) bleaching: be cooled to 80-85 ℃, get liquor natrii hypochloritis 5000ml and evenly be added dropwise in the agitated reactor, the limit edged stirs, and is warming up to 90-92 ℃ after being added dropwise to complete, and continues reaction 4-6 minute;
3) centrifuge washing: open the agitated reactor bottom valve, blowing gets rid of material in centrifuge, after feed liquid dries; The water pH value of using drinking water to wash to flow out to the centrifuge delivery port as 6-7 after, stop to wash, continued centrifugal 10-15 minute; Do not have direct current water to the centrifuge delivery port and flow out, can discharging;
4) granulate: the filter cake of drying send dry house to wait to dry by the fire after granulator 12 orders are granulated;
5) oven dry: baking material personnel should close all openings of all ebullated beds, and the power turn-on switch starts blower fan; Open the thermal source switch, heating; Room temperature to be mixed reaches 100 ℃ of beginning chargings, regulates air-valve, makes the interior material of bed reach best fluidized state; Regulate the thermal source switch, guarantee that the mixing chamber temperature is controlled at 100-120 ℃, 50-60 minute drying time, when material to be dried satisfies drying and requires, discharging; Oven dry finishes, stops earlier heating, room temperature to be mixed drops to 60-80 ℃, stops blower fan, and the material in cleaning bed and the hopper is closed the turnover flitch;
6) pulverize: the material of oven dry evenly advances pulverizer and pulverizes;
7) sieve: the material of pulverizing is crossed 200 orders thickening vibrating screen sub-sieve;
8) secondary is pulverized: screened material is sent into the ultra-fine mechanical crusher of LHJ pulverize once more.
Technique effect of the present invention is: this preparation method is that to carry out certain proportioning be raw material for 30 ~ 40% xylon with purified cotton and hemicellulose level; Adopt the hydrolysis of low concentration watery hydrochloric acid; In hydrolytic process, adding clorox bleaches; Shorten hydrolysis time, pulverize and get through micronizer again after drying is just broken; It is high to make the microcrystalline cellulose water imbibition with the present invention, and water-soluble back viscosity is not stratified greatly, and whiteness is greater than 95, and average grain diameter is less than 5 microns.
The specific embodiment
The present invention realizes that like this method step is:
1) hydrolysis: put the 1300Kg drinking water in agitated reactor, open the technical hydrochloric acid measuring tank, it is 0.15-0.20mol/L that the input technical hydrochloric acid makes acidity; Open and be steam heated to 60-80 ℃, close admission valve, start stirring; With the 50kg purified cotton that is torn into flakelet and 50kg hemicellulose level is that 30 ~ 40% xylon drops in the agitated reactor, and the purified cotton average degree of polymerization is 1600-2000, and whiteness is greater than 85; The xylon whiteness is greater than 85; Feed intake finish after, open steam valve and be warmed up to 100 ℃, under this temperature, be hydrolyzed the reaction 8-10 minute;
2) bleaching: be cooled to 80-85 ℃, get liquor natrii hypochloritis 5000ml and evenly be added dropwise in the agitated reactor, the limit edged stirs, and is warming up to 90-92 ℃ after being added dropwise to complete, and continues reaction 4-6 minute;
3) centrifuge washing: open the agitated reactor bottom valve, blowing gets rid of material in centrifuge, after feed liquid dries; The water pH value of using drinking water to wash to flow out to the centrifuge delivery port as 6-7 after, stop to wash, continued centrifugal 10-15 minute; Do not have direct current water to the centrifuge delivery port and flow out, can discharging;
4) granulate: the filter cake of drying send dry house to wait to dry by the fire after granulator 12 orders are granulated;
5) oven dry: baking material personnel should close all openings of all ebullated beds, and the power turn-on switch starts blower fan; Open the thermal source switch, heating; Room temperature to be mixed reaches 100 ℃ of beginning chargings, regulates air-valve, makes the interior material of bed reach best fluidized state; Regulate the thermal source switch, guarantee that the mixing chamber temperature is controlled at 100-120 ℃, 50-60 minute drying time, when material to be dried satisfies drying and requires, discharging; Oven dry finishes, stops earlier heating, room temperature to be mixed drops to 60-80 ℃, stops blower fan, and the material in cleaning bed and the hopper is closed the turnover flitch;
6) pulverize: the material of oven dry evenly advances pulverizer and pulverizes;
7) sieve: the material of pulverizing is crossed 200 orders thickening vibrating screen sub-sieve;
8) secondary is pulverized: screened material is sent into the ultra-fine mechanical crusher of LHJ pulverize once more.

Claims (1)

1. a toothpaste is used the Preparation of microcrystalline cellulose method, it is characterized in that method step is:
1) hydrolysis: put the 1300Kg drinking water in agitated reactor, open the technical hydrochloric acid measuring tank, it is 0.15-0.20mol/L that the input technical hydrochloric acid makes acidity; Open and be steam heated to 60-80 ℃, close admission valve, start stirring; With the 50kg purified cotton that is torn into flakelet and 50kg hemicellulose level is that 30 ~ 40% xylon drops in the agitated reactor, and the purified cotton average degree of polymerization is 1600-2000, and whiteness is greater than 85; The xylon whiteness is greater than 85; Feed intake finish after, open steam valve and be warmed up to 100 ℃, under this temperature, be hydrolyzed the reaction 8-10 minute;
2) bleaching: be cooled to 80-85 ℃, get liquor natrii hypochloritis 5000ml and evenly be added dropwise in the agitated reactor, the limit edged stirs, and is warming up to 90-92 ℃ after being added dropwise to complete, and continues reaction 4-6 minute;
3) centrifuge washing: open the agitated reactor bottom valve, blowing gets rid of material in centrifuge, after feed liquid dries; The water pH value of using drinking water to wash to flow out to the centrifuge delivery port as 6-7 after, stop to wash, continued centrifugal 10-15 minute; Do not have direct current water to the centrifuge delivery port and flow out, can discharging;
4) granulate: the filter cake of drying send dry house to wait to dry by the fire after granulator 12 orders are granulated;
5) oven dry: baking material personnel should close all openings of all ebullated beds, and the power turn-on switch starts blower fan; Open the thermal source switch, heating; Room temperature to be mixed reaches 100 ℃ of beginning chargings, regulates air-valve, makes the interior material of bed reach best fluidized state; Regulate the thermal source switch, guarantee that the mixing chamber temperature is controlled at 100-120 ℃, 50-60 minute drying time, when material to be dried satisfies drying and requires, discharging; Oven dry finishes, stops earlier heating, room temperature to be mixed drops to 60-80 ℃, stops blower fan, and the material in cleaning bed and the hopper is closed the turnover flitch;
6) pulverize: the material of oven dry evenly advances pulverizer and pulverizes;
7) sieve: the material of pulverizing is crossed 200 orders thickening vibrating screen sub-sieve;
8) secondary is pulverized: screened material is sent into the ultra-fine mechanical crusher of LHJ pulverize once more.
CN201210024162XA 2012-02-04 2012-02-04 Preparation method of microcrystalline cellulose for toothpaste Pending CN102587182A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103864941A (en) * 2013-12-27 2014-06-18 山东光大科技发展有限公司 Method for preparing microcrystalline cellulose for toothpaste
CN106146675A (en) * 2016-08-16 2016-11-23 河南正弘药用辅料有限公司 A kind of microcrystalline Cellulose production technology
CN109528513A (en) * 2018-12-29 2019-03-29 拉芳家化股份有限公司 It is a kind of without abrasion whitening toothpaste

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2978446A (en) * 1957-01-28 1961-04-04 American Viscose Corp Level-off d.p. cellulose products
CN1671743A (en) * 2002-07-26 2005-09-21 Fmc有限公司 Production of microcrystalline cellulose
CN101368347A (en) * 2008-09-12 2009-02-18 王跃成 Technique for producing mlcrocrystalline cellulose by sulfated waste velveteen
CN101481424A (en) * 2009-02-06 2009-07-15 北京大学 Ultra-fine microcrystalline cellulose and preparation thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2978446A (en) * 1957-01-28 1961-04-04 American Viscose Corp Level-off d.p. cellulose products
CN1671743A (en) * 2002-07-26 2005-09-21 Fmc有限公司 Production of microcrystalline cellulose
CN101368347A (en) * 2008-09-12 2009-02-18 王跃成 Technique for producing mlcrocrystalline cellulose by sulfated waste velveteen
CN101481424A (en) * 2009-02-06 2009-07-15 北京大学 Ultra-fine microcrystalline cellulose and preparation thereof

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103864941A (en) * 2013-12-27 2014-06-18 山东光大科技发展有限公司 Method for preparing microcrystalline cellulose for toothpaste
CN106146675A (en) * 2016-08-16 2016-11-23 河南正弘药用辅料有限公司 A kind of microcrystalline Cellulose production technology
CN106146675B (en) * 2016-08-16 2019-01-18 河南正弘药用辅料有限公司 A kind of microcrystalline cellulose production technology
CN109528513A (en) * 2018-12-29 2019-03-29 拉芳家化股份有限公司 It is a kind of without abrasion whitening toothpaste

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Application publication date: 20120718