CN103122592B - Method for preparing microcrystalline cellulose from waste cotton - Google Patents
Method for preparing microcrystalline cellulose from waste cotton Download PDFInfo
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- CN103122592B CN103122592B CN201110369037.8A CN201110369037A CN103122592B CN 103122592 B CN103122592 B CN 103122592B CN 201110369037 A CN201110369037 A CN 201110369037A CN 103122592 B CN103122592 B CN 103122592B
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Abstract
The invention relates to a method for preparing microcrystalline cellulose from waste cotton. The method comprises the following steps of: (1) mixing and contacting the waste cotton with an acid solution to obtain acidified waste cotton; and (2) carrying out contact reaction on the acidified waste cotton and an oxidant at the condition of pH (Potential of Hydrogen) of 2 to 7 in the presence of water. According to the method provided by the invention, the waste cotton can be hydrolyzed and bleached at the same time in one step to obtain the microcrystalline cellulose, and the processes of bleaching and hydrolyzing do not need to be independently carried out, so that the production process of the microcrystalline cellulose can be simplified; and the method is free of high-temperature alkali cooking and degreasing processes, so that the material consumption and the energy consumption in the whole preparation process can be greatly reduced.
Description
Technical field
The present invention relates to a kind of method being prepared microcrystalline cellulose by waste cotton.
Background technology
Waste cotton generally includes cotton waste material that discarded COTTON FABRIC, discarded cotton and cotton produce in the processes such as cotton ginning, lint and weaving (as chimney suede, machine tripe suede, fly suede, fall suede etc.) etc.Although these waste cottons can not be used for cotton spinning, containing a large amount of good fiber quality element, if as offal treatment, both wasted resource, but also serious pollution can be caused to environment.
At present, microcrystalline cellulose has been widely used in the fields such as medicine, food, cosmetics and synthetic leather, such as, excipient and the tablet disintegrant of compressing tablet is used as in medicine, emulsifying agent and foam stabiliser etc. is used as in food processing process, for the production of paste or cosmetics in cosmetics, in synthetic leather manufacture process, be used as tackifier and Micropore Agent etc.
The preparation method of traditional microcrystalline cellulose, such as CN101864684A discloses a kind of method of preparing pharmaceutical-grade microcrystalline cellulose from cotton linter, and the method to comprise cotton linter through boiling degreasing, bleaching purifying, hydrolysis, filtration washing, oven dry, obtains pharmaceutical-grade microcrystalline cellulose after pulverizing.But the technics comparing so preparing microcrystalline cellulose is loaded down with trivial details, need to carry out high-temperature alkali boiling degreasing, material consumption, energy consumption are larger.
Summary of the invention
The invention provides a kind of method being prepared microcrystalline cellulose by waste cotton, the method can not only realize recycling waste cotton, and preparation process is simple, and material consumption, energy consumption are lower.
The invention provides a kind of method being prepared microcrystalline cellulose by waste cotton, the method comprises the following steps:
(1) waste cotton is mixed with acid solution contact, obtain acidified waste cotton;
(2) in presence of water, be under the condition of 2-7 in pH value, described acidified waste cotton and oxidising agent are reacted.
According to described method provided by the invention, under the effect of oxidant, make acidified waste cotton direct hydrolysis and bleaching, thus obtain microcrystalline cellulose, and bleach and hydrolytic process without the need to separately carrying out, thus simplify the production technology of microcrystalline cellulose; And without the need to carrying out high-temperature alkali boiling skimming processes in described method of the present invention, make whole preparation process material consumption, energy consumption lower.
In addition, described method provided by the invention achieves the recycling of waste cotton.
Detailed description of the invention
The method preparing microcrystalline cellulose by waste cotton according to the present invention comprises the following steps:
(1) waste cotton is mixed with acid solution contact, obtain acidified waste cotton;
(2) in presence of water, be under the condition of 2-7 in pH value, described acidified waste cotton and oxidising agent are reacted.
According to described method provided by the invention, in step (1), be the amorphous area making acid solution infiltrated fiber element by the object that described waste cotton mixes with acid solution, with the hydrolysis of accelerating fibers element in subsequent step.In the present invention, described waste cotton and acid solution mix the condition contacted and can comprise: Contact Temperature is 0-90 DEG C, preferred 20-30 DEG C; Contact time is 1 little of 500 days, is preferably 12 little of 10 days.
According to described method provided by the invention, in step (1), the weight ratio of described waste cotton and described acid solution can be 1: 0.001-1, is preferably 1: 0.01-0.8, is more preferably 1: 0.1-0.6; The concentration of described acid solution can be 1-98 % by weight, is preferably 1-30 % by weight.
According to described method provided by the invention, in step (1), the acid in described acid solution can be various routine can the inorganic acid of amorphous area of infiltrated fiber element or organic acid.In the present invention, described inorganic acid can be the inorganic acid of various routine, such as, can be one or more in hydrochloric acid, sulfuric acid, phosphoric acid and nitric acid; Described organic acid can be the organic acid of various routine, and such as carbon number is unitary or the binary organic carboxyl acid of 1-5; Be specifically as follows in formic acid, acetic acid, tartaric acid and citric acid one or more.
According to described method provided by the invention, in step (1), cotton waste material that described waste cotton can produce in cotton ginning, lint and fabrication processes for discarded COTTON FABRIC, discarded cotton and cotton (as chimney suede, machine tripe suede, fly suede, fall suede etc.) at least one.In the present invention, when described waste cotton comprises discarded COTTON FABRIC and/or described discarded cotton, described method of the present invention preferably also comprises to be pulverized described waste cotton, so that the size of described waste cotton is reduced to less than 1 millimeter, is preferably 1-350 μm.
According to described method provided by the invention, in step (1), in order to impel described waste cotton acidifying, described method is preferably also included in described waste cotton to mix in the process contacted with acid solution and adds surfactant and bleeding agent.Described surfactant can be the surfactant of various routine, such as, can be paregal O.Described bleeding agent can be the bleeding agent of various routine, such as, can be penetrant t X-9 or TX-10.Relative to the described waste cotton of 100 weight portions, the addition of described surfactant and bleeding agent can be 0.1-10 weight portion separately.
According to described method provided by the invention, in step (2), be in order to described acidified waste cotton is hydrolyzed and bleaches by the object that described acidified waste cotton and oxidising agent react.In described catalytic process, the pH value of reaction system requires to control in the scope of 2-7.When pH value is too high or too low, easily there is gelatinization and produce colloid in described acidified waste cotton, thus be difficult to generate microcrystalline cellulose.Under preferable case, the pH value of reaction system controls as 3-5.
According to described method provided by the invention, in step (2), the pH value of reaction system can be regulated by the form adding dilute acid soln, and described dilute acid soln can be such as dilution heat of sulfuric acid or dilute hydrochloric acid solution.Under preferable case, when the acid solution used in step (1) is for sulfuric acid solution, the dilute acid soln for adjust ph in step (2) is preferably hydrochloric acid solution.
According to described method provided by the invention, in step (2), the haptoreaction of described acidified waste cotton and described oxidant is preferably carried out in the presence of a catalyst.The enzyme that described catalyst is preferably water-soluble metal salt and/or cotton fiber can be impelled to be hydrolyzed.Relative to the described acidified waste cotton of 100 weight portions, the consumption of described catalyst can be 0.1-10 weight portion, is preferably 0.5-5 weight portion.In the present invention, as described catalyst, described water-soluble metal salt is preferably selected from sulfate or the chloride of at least one metal in copper, iron, zinc and chromium, such as, can be copper chloride, frerrous chloride, zinc chloride, chromium chloride etc.; The described enzyme that cotton fiber can be impelled to be hydrolyzed be preferably in cellulase, laccase, zytase and pectase one or more.
According to described method provided by the invention, in step (2), the condition that described acidified waste cotton and oxidising agent react preferably includes: reaction temperature is 0-100 DEG C, is preferably 35-60 DEG C; Reaction time is 0.1-10 hour, is preferably 1-2 hour.
According to described method provided by the invention, in step (2), relative to the described acidified waste cotton of 100 weight portions, the consumption of described water is 100-10000 weight portion, is preferably 300-1000 weight portion.
According to described method provided by the invention, in step (2), relative to the described acidified waste cotton of 100 weight portions, the consumption of described oxidant is 1-200 weight portion, is preferably 2-15 weight portion.In the present invention, described oxidant is preferably one or more in hydrogen peroxide, clorox, calcium hypochlorite, hydroxyl radical free radical active oxygen and chlorine dioxide.Under further preferable case, described oxidant is clorox.
According to described method provided by the invention, in order to recycle sulfated waste cotton velvet, in step (2), described method is preferably also included in the process of described acidified waste cotton and oxidising agent being reacted and adds sulfated waste cotton velvet.Relative to the described acidified waste cotton of 100 weight portions, the consumption of described sulfated waste cotton velvet can be 0.1-1000 weight portion, is preferably 10-50 weight portion.In the present invention, described sulfated waste cotton velvet refers to the waste acid cotton linter taken off from cottonseed with dilute sulfuric acid in cotton seed production of hybrid seeds process.Usually, described sulfated waste cotton velvet is incinerated for a long time, creates very adverse influence to atmospheric environment.Therefore, by recycling described sulfated waste cotton velvet in the present invention, efficiently avoid the generation of above-mentioned unfavorable factor.
According to one embodiment of the present invention, in order to improve the purity of the microcrystalline cellulose of final preparation further, described method of the present invention to be preferably also included in after above-mentioned steps (1) and before above-mentioned steps (2), described acidified waste cotton is carried out removal of impurities, to remove the large volume impurity in described acidified waste cotton.It is 1: 5-20 to mix that the method for described removal of impurities can to comprise described acidified waste cotton and water with weight ratio, then carries out removal of impurities with conical refiner.
According to another embodiment of the invention, in order to obtain the microcrystalline cellulose of suitable particle size, described method of the present invention preferably also comprise the product obtained after haptoreaction in step (2) carried out dewater, dry and pulverize.The particle size of the microcrystalline cellulose of final preparation can be crushed in different particle size range according to the difference of Application Areas, and usually, being crushed to particle size is 10-400 order.In the present invention, described particle size refers to the mesh size being obtained the screen cloth of this particle by screening.
The invention will be further described with comparative example by the following examples.
Embodiment 1
The present embodiment is for illustration of the described method being prepared microcrystalline cellulose by waste cotton of the present invention.
Dilution heat of sulfuric acid (concentration is 10 % by weight) is sprayed on the chimney suede produced in embossing process by cotton to carry out acidifying to described chimney suede, the weight ratio of described dilution heat of sulfuric acid and described chimney suede is 0.1: 1, carries out acidifying 30 days at normal temperatures to described chimney suede.Afterwards, be carry out mix and blend at 1: 10 by acidified chimney suede and water with weight ratio, then carry out removal of impurities with conical refiner.Then, the cellulase of above-mentioned the chimney suede, the water of 200 weight portions, the clorox of 10 weight portions and 5 weight portions that obtain after removal of impurities of 100 weight portions is added in reactor, and by concentration be 10 % by weight hydrochloric acid solution the pH value of the mixed material in reactor is adjusted to 5, make this mixture insulation reaction 10 hours at 40 DEG C afterwards, obtain slurries.Then, carried out successively by these slurries dewatering, dry and pulverize, obtaining particle size is 80 object microcrystalline celluloses.
The purity recording this microcrystalline cellulose according to the method for GB/T744-1989 is 95%; The whiteness recording this microcrystalline cellulose through WSB-II d/o whiteness instrument is 75.
Embodiment 2
The present embodiment is for illustration of the described method being prepared microcrystalline cellulose by waste cotton of the present invention.
According to microcrystalline cellulose prepared by the method for embodiment 1, difference is, replaces cellulase with the laccase of identical weight, thus obtained microcrystalline cellulose.
The purity recording this microcrystalline cellulose according to the method for GB/T744-1989 is 96%; The whiteness recording this microcrystalline cellulose through WSB-II d/o whiteness instrument is 77.
Embodiment 3
The present embodiment is for illustration of the described method being prepared microcrystalline cellulose by waste cotton of the present invention.
According to microcrystalline cellulose prepared by the method for embodiment 1, difference is, replaces cellulase with the zytase of identical weight, thus obtained microcrystalline cellulose.
The purity recording this microcrystalline cellulose according to the method for GB/T744-1989 is 95%; The whiteness recording this microcrystalline cellulose through WSB-II d/o whiteness instrument is 74.
Embodiment 4
The present embodiment is for illustration of the described method being prepared microcrystalline cellulose by waste cotton of the present invention.
According to microcrystalline cellulose prepared by the method for embodiment 1, difference is, replaces cellulase with the pectase of identical weight, thus obtained microcrystalline cellulose.
The purity recording this microcrystalline cellulose according to the method for GB/T744-1989 is 96%; The whiteness recording this microcrystalline cellulose through WSB-II d/o whiteness instrument is 75.
Embodiment 5
According to microcrystalline cellulose prepared by the method for embodiment 1, difference is, in described reactor, do not add cellulase, thus obtained microcrystalline cellulose.
The purity recording this microcrystalline cellulose according to the method for GB/T744-1989 is 91%; The whiteness recording this microcrystalline cellulose through WSB-II d/o whiteness instrument is 69.
Comparative example 1
According to microcrystalline cellulose prepared by the method for embodiment 1, difference is, the pH value of the mixed material in described reactor is adjusted to 1, thus obtained microcrystalline cellulose.
The purity recording this microcrystalline cellulose according to the method for GB/T744-1989 is 71%; The whiteness recording this microcrystalline cellulose through WSB-II d/o whiteness instrument is 65.
Embodiment 6
The present embodiment is for illustration of the described method being prepared microcrystalline cellulose by waste cotton of the present invention.
Discarded COTTON FABRIC is crushed to the cotton fiber powder that average particle size particle size is about 1-10 millimeter, then 3 % by weight acetic acid solutions are sprayed on this cotton fiber powder to carry out acidifying to it, the weight ratio of described acetic acid solution and described cotton fiber powder is 0.8: 1, at 20 DEG C, carry out acidifying 50 days to described cotton fiber powder.Afterwards, be carry out mix and blend at 1: 10 by acidified cotton fiber powder and water with weight ratio, then carry out removal of impurities with conical refiner.Then, the frerrous chloride of above-mentioned the cotton fiber powder, the sulfated waste cotton velvet (sulfuric acid content is 5 % by weight) of 20 weight portions, the water of 200 weight portions, the hydrogen peroxide (concentration is 27.5 % by weight) of 5 weight portions and 0.1 weight portion that obtain after removal of impurities that add 80 weight portions in reactor, and by concentration be 10 % by weight hydrochloric acid solution the pH value of the mixed material in reactor is adjusted to 4, make this mixture insulation reaction 3 hours at 50 DEG C afterwards, obtain slurries.Then, carried out successively by these slurries dewatering, dry and pulverize, obtaining particle size is 80 object microcrystalline celluloses.
The purity recording this microcrystalline cellulose according to the method for GB/T744-1989 is 92%; The whiteness recording this microcrystalline cellulose through WSB-II d/o whiteness instrument is 70.
Embodiment 7
The present embodiment is for illustration of the described method being prepared microcrystalline cellulose by waste cotton of the present invention.
According to microcrystalline cellulose prepared by the method for embodiment 5, difference is, replaces frerrous chloride with the copper chloride of identical weight, thus obtained microcrystalline cellulose.
The purity recording this microcrystalline cellulose according to the method for GB/T744-1989 is 90%; The whiteness recording this microcrystalline cellulose through WSB-II d/o whiteness instrument is 70.
Embodiment 8
The present embodiment is for illustration of the described method being prepared microcrystalline cellulose by waste cotton of the present invention.
According to microcrystalline cellulose prepared by the method for embodiment 5, difference is, replaces frerrous chloride with the chromium chloride of identical weight, thus obtained microcrystalline cellulose.
The purity recording this microcrystalline cellulose according to the method for GB/T744-1989 is 89%; The whiteness recording this microcrystalline cellulose through WSB-II d/o whiteness instrument is 69.
Embodiment 9
The present embodiment is for illustration of the described method being prepared microcrystalline cellulose by waste cotton of the present invention.
Discarded cotton is crushed to the cotton fiber powder that average particle size particle size is about 1-10 millimeter, then 5 % by weight hydrochloric acid solutions are sprayed on this cotton fiber powder to carry out acidifying to it, the weight ratio of described dilute hydrochloric acid solution and described cotton fiber powder is 0.5: 1, at 25 DEG C, carry out acidifying 100 days to described cotton fiber powder.Afterwards, be carry out mix and blend at 1: 10 by acidified cotton fiber powder and water with weight ratio, then carry out removal of impurities with conical refiner.Then, the cellulase of above-mentioned the cotton fiber powder, the water of 200 weight portions, the chlorine dioxide of 15 weight portions and 2 weight portions that obtain after removal of impurities of 100 weight portions is added in reactor, and by concentration be 10 % by weight hydrochloric acid solution the pH value of the mixed material in reactor is adjusted to 3, make this mixture insulation reaction 2 hours at 55 DEG C afterwards, obtain slurries.Then, carried out successively by these slurries dewatering, dry and pulverize, obtaining particle size is 80 object microcrystalline celluloses.
The purity recording this microcrystalline cellulose according to the method for GB/T744-1989 is 94%; The whiteness recording this microcrystalline cellulose through WSB-II d/o whiteness instrument is 75.
According to the record of above-described embodiment and comparative example, particularly embodiment 1 and comparative example 1 are compared and can be found out, method according to the present invention can obtain higher purity and the microcrystalline cellulose of whiteness.
Above detailed description of the invention is only for describing the preferred embodiment of the present invention; but; the present invention is not limited to the detail in above-mentioned embodiment; within the scope of technical conceive of the present invention; can carry out multiple simple variant to technical scheme of the present invention, these simple variant all belong to protection scope of the present invention.
Claims (12)
1. prepared a method for microcrystalline cellulose by waste cotton, the method comprises the following steps:
(1) waste cotton is mixed with acid solution contact, obtain acidified waste cotton;
(2) in presence of water, be under the condition of 2-7 in pH value, described acidified waste cotton and oxidising agent are reacted; Wherein, described haptoreaction is carried out in the presence of a catalyst, the enzyme that described catalyst is water-soluble metal salt and/or cotton fiber can be impelled to be hydrolyzed.
2. method according to claim 1, wherein, in step (1), the condition of described mixing contact comprises: Contact Temperature is 0-90 DEG C, and soak time is 1 little of 500 days.
3. method according to claim 1, wherein, in step (1), the weight ratio of described waste cotton and described acid solution is 1:0.001-1, and the concentration of described acid solution is 1-98 % by weight.
4. the method according to claim 1 or 3, wherein, in step (1), acid in described acid solution is inorganic acid or organic acid, described inorganic acid is one or more in hydrochloric acid, sulfuric acid, phosphoric acid and nitric acid, and described organic acid is one or more in formic acid, acetic acid, tartaric acid and citric acid; Described waste cotton is at least one in the velveteen waste material that produces in cotton ginning, lint and fabrication processes of discarded COTTON FABRIC, discarded cotton and cotton.
5. method according to claim 1, wherein, described water-soluble metal salt is sulfate or the chloride of at least one metal be selected from copper, iron, zinc and chromium; Described enzyme is at least one in cellulase, laccase, zytase and pectase.
6. method according to claim 1, wherein, in step (2), described catalytic condition comprises: reaction temperature is 0-100 DEG C, and the reaction time is 0.1-10 hour.
7. method according to claim 6, wherein, in step (2), described catalytic condition comprises: reaction temperature is 35-60 DEG C, and the reaction time is 1-2 hour.
8. method according to claim 1, wherein, in step (2), pH value is 3-5.
9. method according to claim 1, wherein, in step (2), relative to the described acidified waste cotton of 100 weight portions, the consumption of described water is 100-1000 weight portion, and the consumption of described oxidant is 1-200 weight portion, and the consumption of described catalyst is 0.1-10 weight portion.
10. the method according to claim 1 or 9, wherein, in step (2), described oxidant is one or more in hydrogen peroxide, clorox, calcium hypochlorite, hydroxyl radical free radical active oxygen and chlorine dioxide.
11. methods according to claim 1, wherein, in step (2), described method is also included in the process that described acidified waste cotton and oxidising agent react and adds sulfated waste cotton velvet, relative to the described acidified waste cotton of 100 weight portions, the consumption of described sulfated waste cotton velvet is 0.1-1000 weight portion.
12. methods according to claim 11, wherein, relative to the described acidified waste cotton of 100 weight portions, the consumption of described sulfated waste cotton velvet is 10-50 weight portion.
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| CN105064110B (en) * | 2015-07-29 | 2017-04-12 | 华南理工大学 | Cotton linter pulping device and pulping method thereof |
| CN105019286B (en) * | 2015-07-29 | 2017-01-25 | 华南理工大学 | Device and method for making refined cottons through performing high-concentration hydrogen peroxide bleaching on cotton linters |
| CN106986946A (en) * | 2017-04-10 | 2017-07-28 | 华纺股份有限公司 | A kind of cotton noils prepares microcrystalline cellulose technique |
| CN108505374B (en) * | 2018-04-22 | 2019-11-08 | 江苏源清环保科技有限公司 | A kind of preparation method of modified cellulose insulating paper |
| CN108547079B (en) * | 2018-06-08 | 2023-10-10 | 北京鹏盛天纤科技有限公司 | Green continuous production integrated device and process for absorbent cotton |
| CN113388652B (en) * | 2021-07-07 | 2023-04-28 | 西南林业大学 | Preparation method of green efficient nanocellulose |
| CN117285311B (en) * | 2023-08-30 | 2024-08-20 | 泰山石膏(菏泽)有限公司 | Waterproof and fireproof multifunctional paper-faced gypsum board and preparation method thereof |
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| CN1220271A (en) * | 1997-10-13 | 1999-06-23 | 徐旗开 | Method for producing microcrystalline cellulose by sulfating waste cotton velvet |
| CN101368347A (en) * | 2008-09-12 | 2009-02-18 | 王跃成 | Technique for producing mlcrocrystalline cellulose by sulfated waste velveteen |
| CN102080346A (en) * | 2010-11-25 | 2011-06-01 | 山东轻工业学院 | Application of cation nano microcrystalline cellulose as paper reinforcing agent |
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| CN1081185A (en) * | 1992-07-04 | 1994-01-26 | 苏志刚 | Use technology for producing microcrystalline cellulose with sulfated waste cotton velvet |
| CN1220271A (en) * | 1997-10-13 | 1999-06-23 | 徐旗开 | Method for producing microcrystalline cellulose by sulfating waste cotton velvet |
| CN101368347A (en) * | 2008-09-12 | 2009-02-18 | 王跃成 | Technique for producing mlcrocrystalline cellulose by sulfated waste velveteen |
| CN102080346A (en) * | 2010-11-25 | 2011-06-01 | 山东轻工业学院 | Application of cation nano microcrystalline cellulose as paper reinforcing agent |
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