CN103087204B - Micro-powder cellulose preparation method - Google Patents
Micro-powder cellulose preparation method Download PDFInfo
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- CN103087204B CN103087204B CN201110332825.XA CN201110332825A CN103087204B CN 103087204 B CN103087204 B CN 103087204B CN 201110332825 A CN201110332825 A CN 201110332825A CN 103087204 B CN103087204 B CN 103087204B
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Abstract
The invention discloses a micro-powder cellulose preparation method, which is characterized in that cotton dust is adopted as a raw material, purity-increase impurity-removing and decoloration degradation are performed, and one of an improved twin-screw slurry extruder, a ball mill, a rod mill and a vibration mill is adopted to carry out a high shear oxidation depolymerization treatment to obtain the micro-powder cellulose, wherein cotton dust can not be used by textile industry. According to the present invention, the characteristic of low polymerization degree of the cotton dust fine fiber is utilized, and the resource is complete, such that large-scale industrial production can be performed, and product stability and purity are high.
Description
Technical field
The present invention relates to a kind of method of micro-powder cellulose preparation.
Background technology
Micro mist (crystallite) Mierocrystalline cellulose is cellulosic a kind of new form, is that cellulose materials is through being hydrolyzed reach capacity a kind of high dispersion of polymerization degree generation and the micron powder shape product of adsorptivity.In recent years, the exploitation of powdered celluloses is extremely paid attention to research, and has been widely used in the fields such as leather, welding rod, food, medicine, building materials and household chemicals.But because of current domestic micro-powder cellulose preparation mainly by natural cellulose (purified cotton or high-quality wood pulp) through dilute acid hydrolysis to levelling-off DP, then to produce through the technique of suitable mechanical treatment.High-quality cotton pulp, pulp sources that the method consumption is a large amount of, and producing a large amount of waste water with in acid hydrolysis production process, affect environment.Due to above reason, the state that current domestic main manufacturer majority is on a small scale and dispersion is produced, seriously constrains the development of China's powdered celluloses industry.
Prior art is generally carries out acidification hydrolization by Mierocrystalline cellulose, and cost is higher.Cotton fibre is the vegetable fibre of occurring in nature natural fiber cellulose content the highest (containing more than 95%).The method selects cotton dirt to be principle.Cotton dirt refers to that the waste that the cotton fiber fines flying dust that cotton and textile process enterprise produce in process of production focuses on recovery through dust collecting process " spends dirt ", annual generation about 400,000 tons of cotton dirt according to relevant statistics.Be cotton fiber fines powder (more than 90%) for " cotton dirt " main component, the polymerization degree low (about 500), the feature that impurity is many, ash content is high, can turn waste into wealth after taking the process of the technology of the present invention technology and equipment.
Sum up above-mentioned, adopt cotton dirt fiber fines to prepare powdered celluloses and greatly will save cost, there is high economic and social benefit.
Summary of the invention
The invention provides a kind of method of micro-powder cellulose preparation, with cotton " cotton dirt " i.e. cotton fiber fines for raw material, employing high shear oxidation depolymerization process, solves the problem of the wasting of resources, environmental pollution and industrial mass production.
The present invention is realized by following technical scheme:
A method for micro-powder cellulose preparation is realized by following step:
(1) cotton dirt defecation removal of impurities: adopt gradation sizing equipment to carry out the removal of impurities of dry method defecation the cotton dirt raw material reclaimed, remove portion can be used for cotton fibre and the part non-fiber impurity of paper pulp;
(2) cotton fibre decolored degradation: by purify after cotton dirt and industrial hydrogen peroxide solution carry out being stirred to cotton dirt oven dry stock content be 68% ~ 73% time, adding another kind of oxidizing solution again carries out being stirred to cotton dirt oven dry stock content when being 48% ~ 53%, carries out high shear oxidation depolymerization process and obtains cellulose materials;
(3) Mierocrystalline cellulose is refined: the cellulose materials after abundant depolymerization carried out washing impurity-removing, dehydrates afterwards, grind classification or naturally dry and directly grind classification after moisture 15%.
In described step (2), industrial hydrogen peroxide solution is hydrogen peroxide 5 ~ 15%.
In described step (2), another kind of oxidizing solution is the mixture of following solutions: NaOH 1% ~ 3%, NaSiO
31.5 ~ 2.5%, the 25 kilograms of proportioning mixing of the cotton dirt after DTPA 0.13% ~ 0.18%, the every 100 kilograms of described purifications of water.
In described step (2), the overall churning time of oven dry stock is 30 minutes.
In described step (2), high shear oxidation depolymerization process adopts the one in twin screw pulp-extruding machine, ball mill, rod mill, vibration mill.
Washing impurity-removing is add described 2 ~ 3% vitriol oils of Mierocrystalline cellulose oven dry stock gross weight and the water of 100 parts to form dilute sulfuric acid aqueous solution and fully stir removal of impurities in described step (3), then be washed with water to when pH is 7 with industry and remove the gred, to ash content below 1%.
Dehydrate in described step (3) for by cellulose materials dehydration be 40% to water-content time, dry, dry to Mierocrystalline cellulose water-content be less than 5% ~ 15% terminate.
A kind of method of micro-powder cellulose preparation, the method of described a kind of micro-powder cellulose preparation is a kind of method preparing leather fiber fill element micro mist, be specially: the cellulose materials after abundant depolymerization is carried out nature in described Mierocrystalline cellulose treating process and dry after to moisture 15% and directly grind classification, carry out ground 200 ~ 325 eye mesh screens and divide grade packaged.
Beneficial effect of the present invention is:
1, the present invention is directed to the low feature of the abundant polymerization degree of cotton dust resources used, the depolymerization reaction taking high shear treatment to carry out is oxidizing reaction instead of acidolysis reaction, therefore can save great lot of water resources and reduce pollution.
2, creativeness solves the bottleneck producing micro mist (crystallite) cellulosic material and production method, can save a large amount of high-quality cotton, paper pulp resource, reduces the production cost of the industries such as leather, welding rod, building materials and can realize large-scale industrial production.
3, micro mist (crystallite) Mierocrystalline cellulose utilizing the present invention to produce, whiteness (ISO) can reach 70% ~ 85%, fineness 80 order ~ 600 order is adjustable, and ash content can be controlled within 0.5% ~ 5%, its stability and the complete alternative product utilizing cotton pulp and wood pulp production at present of purity.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention
Fig. 2 is a kind of schema producing leather powdered celluloses
1-dust, 2-blower fan, 3-is except sandbox, and 4-cyclonic separator, 5-divides grit chamber, 6-liquid pool (liquid pool A, liquid pool B), and 7-kneader, 8-dries, 9-shredder, the packing of 10-finished product
Embodiment
Below in conjunction with accompanying drawing, the present invention will be further described.
As Fig. 1, be process flow sheet of the present invention, be specially:
(1) cotton dirt defecation removal of impurities: blast except sandbox 3 by blower fan 2 by the cotton dirt raw material 1 reclaimed, is removing particle diameter larger sand one class non-fiber impurity in sandbox 3.Cotton dirt raw material after desanding passes into cyclonic separator 4, by non-fiber magazins' layout such as cotton leaves, enter granulated slag room 5, cotton dirt starting material left is the tiny cotton fibre of the polymerization degree less than 500, in the impurity wherein removed, the cotton fibre of the polymerization degree higher (more than 800) containing cotton dirt total amount about 5%, can reclaim as paper pulp linters raw material.
(2) cotton fibre decolored degradation: the cotton dirt after purifying is passed into kneader 7, and liquid pool 6 is divided into A, B, C tri-Room, configures hydrogen peroxide 5%-15% (oven dry stock content) mixing solutions, configure NaOH 1% ~ 3%, NaSiO in B in A
31.5 ~ 2.5%, DTPA 0.13% ~ 0.18%, the 25 kilograms of proportioning mixing of cotton dirt after the every 100 kilograms of described purifications of water, after the cotton dirt after purifying passes into kneader 7, A room solution is controlled to pass into kneader 7, when to be stirred to cotton dirt oven dry stock content be about 68% ~ 73%, B room solution is controlled to pass into kneader 7, being stirred to cotton dirt oven dry stock content is about 48% ~ 53%, controlling overall churning time is input twin screw pulp-extruding machine more afterwards in 30 minutes, ball mill, rod mill, one in vibration mill carries out high shear oxidation depolymerization process, obtain the cellulose materials of oxidative decoloration, if need refining reduction ash content further, the cellulose materials obtained is passed into little stock tank 9.
(3) Mierocrystalline cellulose is refined:
A, washing impurity-removing: in the C room of liquid pool 6, configure industrial molten sulfur acid solution, sulfuric acid in C room is passed into little stock tank 9, intake is 2 ~ 3% of fiber oven dry stock weight, wherein sulfuric acid is that the water of 2 ~ 3% vitriol oils and 100 parts forms dilute sulfuric acid aqueous solution and fully stirs removal of impurities, then be washed with water to when pH is 7 with industry and remove the gred, to ash content below 1%, add water and be uniformly mixed Mierocrystalline cellulose that rear conveying need refine and fully stir that within 30 minutes, to form content of cellulose be the slurries of about 15%, sulfuric acid can remove calcium, magnesium, sodium, potassium, silicon, iron, the ash contents such as copper, and product whiteness can be improved further.The filamentary material processed delivers to drainer 12 by mashing pump 10, and process water is passed into drainer 12 by water softener tank 11, washs when reaching 7 to pH, removes the gred.Remove the gred as secondary removes the gred, namely first remove grit chamber 13 by one-level, then by secondary except grit chamber 14, two-stage slag removal falls into the bits except grit chamber 17, carry out secondary slagging-off recovery if also can return containing part cotton fibre.
B, to dehydrate: enter vacuum hydroextractor 15 through the filamentary material of two-stage slag removal and concentrate, dehydration passes into baker 16 to when being 40% containing cotton fibre rate, inlet temperature is set to 90 ~ 130 DEG C, and discharge port temperature is 60 DEG C, dries and is less than 15% to cotton fibre particle is moisture.
C, grinding classification: above-mentioned materials is passed into shredder 18, sieve after requiring to be ground to 80 ~ 350 orders, finally carry out finished product packing 19 operation, complete preparation according to user.
As Fig. 2, according to above-mentioned method, leather filling powdered celluloses can be prepared, have in figure known, the cellulosic material of depolymerization of decolouring in kneader 7 is carried out nature when drying 8 to water content about 15%, enter shredder 9 and process rear mistake 200 ~ 325 order mesh screen and carry out finished product classification 10.
Claims (7)
1. a method for micro-powder cellulose preparation, it is characterized in that by following step realize:
(1) cotton dirt defecation removal of impurities: adopt gradation sizing equipment to carry out the removal of impurities of dry method defecation the cotton dirt raw material reclaimed, remove portion can be used for cotton fibre and the part non-fiber impurity of paper pulp;
(2) cotton fibre decolored degradation: by purify after cotton dirt and industrial hydrogen peroxide solution carry out being stirred to cotton dirt oven dry stock content be 68% ~ 73% time, adding another kind of oxidizing solution again carries out being stirred to cotton dirt oven dry stock content when being 48% ~ 53%, carries out high shear oxidation depolymerization process and obtains cellulose materials;
(3) Mierocrystalline cellulose is refined: the cellulose materials after abundant depolymerization carried out washing impurity-removing, dehydrates afterwards, grind classification or naturally dry and directly grind classification after moisture 15%;
In described step (2), another kind of oxidizing solution is the mixture of following solutions: NaOH1% ~ 3%, NaSiO
31.5 ~ 2.5%, the 25 kilograms of proportioning mixing of the cotton dirt after DTPA 0.13% ~ 0.18%, the every 100 kilograms of described purifications of water.
2. the method for a kind of micro-powder cellulose preparation as claimed in claim 1, is characterized in that in described step (2), industrial hydrogen peroxide solution is hydrogen peroxide 5 ~ 15%.
3. the method for a kind of micro-powder cellulose preparation as claimed in claim 1, is characterized in that in described step (2), the overall churning time of oven dry stock is 30 minutes.
4. the method for a kind of micro-powder cellulose preparation as claimed in claim 1, is characterized in that in described step (2), high shear oxidation depolymerization process adopts the one in twin screw pulp-extruding machine, ball mill, rod mill, vibration mill.
5. the method for a kind of micro-powder cellulose preparation as claimed in claim 1, to it is characterized in that in described step (3) that washing impurity-removing is add described 2 ~ 3% vitriol oils of Mierocrystalline cellulose oven dry stock gross weight and the water of 100 parts to form dilute sulfuric acid aqueous solution and fully stir removal of impurities, then be washed with water to when pH is 7 with industry and remove the gred, to ash content below 1%.
6. the method for a kind of micro-powder cellulose preparation as claimed in claim 1, when it is characterized in that dehydrating in described step (3) as being 40% by cellulose materials dehydration to water-content, dry, dry to Mierocrystalline cellulose water-content be less than 5% ~ 15% terminate.
7. as the method for a kind of micro-powder cellulose preparation in Claims 1 to 4 as described in any one claim, it is characterized in that the method for described a kind of micro-powder cellulose preparation is a kind of method preparing leather fiber fill element micro mist, be specially: the cellulose materials after abundant depolymerization is carried out nature in described Mierocrystalline cellulose treating process and dry after to moisture 15% and directly grind classification, carry out ground 200 ~ 325 eye mesh screens and divide grade packaged.
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| CN201110332825.XA CN103087204B (en) | 2011-10-28 | 2011-10-28 | Micro-powder cellulose preparation method |
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| CN201110332825.XA CN103087204B (en) | 2011-10-28 | 2011-10-28 | Micro-powder cellulose preparation method |
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| CN103319730A (en) * | 2013-05-30 | 2013-09-25 | 清丰同化新材料科技有限公司 | Preparation method of lignocellulose for synthetic leather |
| CN107446058B (en) * | 2017-06-23 | 2019-08-16 | 广西大学 | A kind of preparation method and applications of nanometer of manioc waste |
| CN113417164A (en) * | 2021-07-27 | 2021-09-21 | 湖州市菱湖新望化学有限公司 | Production method of powdery cellulose |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101067287A (en) * | 2007-05-31 | 2007-11-07 | 王光建 | Producing technology for microcrystalline cellulose with waste acid cotton linter |
| CN101302725A (en) * | 2008-06-10 | 2008-11-12 | 山东银鹰化纤有限公司 | Process for producing cotton dissolving pulp |
| CN101775161A (en) * | 2009-01-12 | 2010-07-14 | 四川省蓬溪县弘桥实业有限公司 | Process for producing modified starch by using microwave far infrared method |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101067287A (en) * | 2007-05-31 | 2007-11-07 | 王光建 | Producing technology for microcrystalline cellulose with waste acid cotton linter |
| CN101302725A (en) * | 2008-06-10 | 2008-11-12 | 山东银鹰化纤有限公司 | Process for producing cotton dissolving pulp |
| CN101775161A (en) * | 2009-01-12 | 2010-07-14 | 四川省蓬溪县弘桥实业有限公司 | Process for producing modified starch by using microwave far infrared method |
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