CN101368347B - Technique for producing mlcrocrystalline cellulose by sulfated waste velveteen - Google Patents
Technique for producing mlcrocrystalline cellulose by sulfated waste velveteen Download PDFInfo
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- CN101368347B CN101368347B CN2008100729533A CN200810072953A CN101368347B CN 101368347 B CN101368347 B CN 101368347B CN 2008100729533 A CN2008100729533 A CN 2008100729533A CN 200810072953 A CN200810072953 A CN 200810072953A CN 101368347 B CN101368347 B CN 101368347B
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- alkali
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- waste cotton
- sulfated
- cotton velvet
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Abstract
The invention discloses a process method which adopts sulfated waste velveteen to produce microcrystalline, mainly including the following steps: measuring and detecting, quantitative neutralization, bleaching, washing, drying, crashing and sieving. The process method is characterized in that in the measuring and detecting process, first, the proportion of alkali used to neutralize sulfated wastevelveteen is detected, then alkali solution is prepared according to the proportion and quantitative sulfated waste velveteen is added for quantitative neutralization, and finally the bleaching process is carried out. Compared with the prior art, the process method requires less energy to process the sulfated waste velveteen; particularly, the proportioning measurement is adopted to determine theamount of waste velveteen and alkali, which reduces the amount of used alkali to the minimum while sufficiently ensuring the quality of the microcrystalline cellulose and greatly reducing production cost. The discharge liquid is neutral or approximately neutral and has little pollution to the environment. On the other hand, the water amount used during neutralization is small, the total dischargeliquid is small in amount and is easy to be disposed without pollution, and the cost is also greatly reduced.
Description
Technical field
The present invention relates to a kind of technology for producing microcrystalline cellulose with sulfated waste cotton velvet method of using.
Technical background
China is one and produces cotton big country, and the sulfated waste cotton velvet of discharging in the cotton seed processing is in the past all made refuse and handled, and processing method mainly is to burn, and has both needed to drop into disposal cost, has wasted human and material resources, and financial resources have caused the pollution to atmosphere again.Chinese patent CN1081185A discloses and has used technology for producing microcrystalline cellulose with sulfated waste cotton velvet, process such as adopt that mainly high temperature neutralization, degraded bleachs, dried, pulverize, sieve, this technology exist energy consumption too high with the stable inadequately defective of quality.The disclosed production method of making microcrystalline cellulose with sulfated waste cotton velvet of Chinese patent CN1220271A, successively by ageing, washing, removal of impurities, bleaching, dechlorination, dewatered drying, pulverize, technical process such as sieve, particularly neutralize and promptly bleach by direct washing, dechlorination, as acid being rinsed well fully, water resource is expended huge, acid pickle after the flushing such as direct discharging meeting cause severe contamination to environment, as wash deficiency and then just have residual acid and exist, use solution such as clorox or calcium hypochlorite to bleach this moment, the bleaching agent effectiveness that residual acid makes in the sulfated waste cotton velvet is difficult to play a role, bleaching effect is had a greatly reduced quality, when calcium hypochlorite or clorox reacted with dilute sulfuric acid, its reaction was:
Ca(ClO)
2+CaCl
2+2H
2SO
4＝2CaSO
4+2Cl
2↑+2H
2O
NaClO+NaCl+H
2SO
4＝Na
2SO
4+Cl
2↑+H
2O
Have a large amount of chlorine dischargings, handle bad meeting serious harm health.
Summary of the invention:
At the problems referred to above, the object of the present invention is to provide a kind of energy consumption and water resource to expend lower, the stay-in-grade technology for producing microcrystalline cellulose with sulfated waste cotton velvet method of using.
The present invention mainly is made up of following technical process: metering detection, quantitatively neutralization, bleaching, cleaning, oven dry, crushing screening operation are characterized in:
Described metering detects: the sulfated waste cotton velvet of getting a weight portion immerses in 5～15 weight parts waters and fully stirred 15～30 minutes, quantitatively also divide at least twice to add alkali: one or both in NaOH, sodium carbonate, the calcium hydroxide, and the acidity of test mixing liquid at any time, up to ph value of mixture is 5～10, be preferably pH value=7～8, write down the amount that every weight parts water should add alkali;
Described quantitatively in and operation be: get 5～15 weight parts waters by 1 weight portion sulfated waste cotton velvet, detect in the alkali that the resulting amount that should add alkali adds metering checkout program in proportion one or both by metering, stir and fully dissolving, during fully stirring, the adding sulfated waste cotton velvet, enters bleaching process after filtering then and drying with 1 ~ 7 hour;
As further improvement, in the process of the quantitative adding alkali that above-mentioned metering detects, reach the alkali number that adds test later on for the second time and can be compared to most the first time of minimizing one by one.
Sulfated waste cotton velvet after the above-mentioned neutralization dries after preferably removing impurity, and described drying is preferably to moisture≤20%.
As improved technical scheme, it is following a kind of that described bleaching process is preferably:
Velveteen after the neutralization is immersed the mixed solution that concentration expressed in percentage by weight is 3～10% liquor natrii hypochloritises or clorox, sodium chloride, soaked 2～7 hours; Perhaps successively immerse in weight percent concentration 1～3% sodium hydroxide solution and 1～3% sodium carbonate liquor and be heated to 60～80 ℃ each 3～10 hours, the liquor natrii hypochloritis with weight percent concentration 1～3% soaked 5～7 hours down for 45～60 ℃ in temperature afterwards.
Described baking operation: dry to moisture 5～10%, described oven dry is preferably steaming process more than 100 ℃, and temperature is preferably at 100 ~ 120 ℃.
Compare with existing technology, the handled sulfated waste cotton velvet energy consumption of the present invention reduces greatly, has particularly adopted metering-type proportioning waste cotton velvet and has thrown alkali number, can make the throwing alkali number drop to minimum, and fully guarantee the quality of gained microcrystalline cellulose to reduce production costs greatly, the waste liquid of discharge be neutral or or near neutral, environmental pollution is little, on the other hand, in and time institute's water consumption few, its waste liquid total amount is few, do not have the dirtization processing and also be easier to, cost also can reduce greatly.
The specific embodiment:
Embodiment 1:
The sulfated waste cotton velvet of getting 1Kg immerses in the 5Kg water and fully stirred 30 minutes, quantitatively add NaOH several times, add 10g at every turn, adding the back stirred 30 minutes, the acidity of mixed liquor behind the each adding of the test alkali, greater than 7, get that time up to ph value of mixture, write down the ratio that every Kg water should add the amount of alkali near 7; With the 5mm sieve big the mixing in the sulfated waste cotton velvet removed earlier, in 1 weight portion sulfated waste cotton velvet: the ratio water intaking of 5 weight parts waters, detect the resulting amount that should add alkali by metering and add NaOH in proportion, stir and fully dissolving, add sulfated waste cotton velvet fully stir in and 3 hours, filter and dry with aperture 75 μ m sieve then to moisture and be lower than 25%, it is 6% liquor natrii hypochloritis's solution that velveteen after the neutralization is immersed concentration expressed in percentage by weight, soaked 3 hours, filter and dry with aperture 75 μ m sieve then to moisture and be lower than 25%, extremely neutral with the clear water washing, pH value is between 6.5～8, insert under 105 ℃ of steam and dry, pulverized the sieve in 250 μ m apertures to moisture≤10%.
Sulfated waste cotton velvet raw material for each batch can once be tested, and the raw material of this batch can be reused according to the data that detect for the first time afterwards.
Embodiment 2:
The sulfated waste cotton velvet of getting 1Kg immerses in the 8Kg water and fully stirred 20 minutes, quantitatively add calcium hydroxide several times, add for the first time 30g, add 15g afterwards at every turn, all stirred 30 minutes after each the adding, test is each to add the acidity of mixed liquor behind the alkali, up to ph value of mixture greater than 7, get that time, write down the ratio that every Kg water should add the amount of alkali near 7; With the 3mm sieve big the mixing in the sulfated waste cotton velvet removed earlier, in 1 weight portion sulfated waste cotton velvet: the ratio water intaking of 8 weight parts waters, detect the resulting amount that should add alkali by metering and add calcium hydroxide in proportion, stir and fully dissolving, add sulfated waste cotton velvet fully stir in and 3 hours, filter and dry with aperture 75 μ m sieve then to moisture and be lower than 25%, immerse and be heated to 70 ℃ of slow stirrings respectively 3 hours in weight percent concentration 2% sodium hydroxide solution, filter and dry to moisture with aperture 75 μ m sieve and be lower than 25%, immerse 2% sodium carbonate liquor again and be heated to 70 ℃ of slow stirrings 3 hours, filter and dry to moisture with aperture 75 μ m sieve and be lower than 25%, liquor natrii hypochloritis with weight percent concentration 3% soaked 5 hours down for 45 ℃ in temperature afterwards, filter and dry to moisture with aperture 75 μ m sieve and be lower than 25%, extremely neutral with the clear water washing, pH value is between 6.6～7.1, insert under 110 ℃ of steam and dry, pulverized the sieve in 250 μ m apertures to moisture≤5%.
Embodiment 3:
The sulfated waste cotton velvet of getting 1Kg immerses in the 15Kg water and fully stirred 15 minutes, quantitatively add NaOH several times, add for the first time 50g, for the second time add 30g, add 10g afterwards at every turn, all stirred 20 minutes after each the adding, the acidity of mixed liquor behind the each adding of the test alkali, greater than 7, get that time up to ph value of mixture, write down the ratio that every Kg water should add the amount of alkali near 7; With the 1.5mm sieve big the mixing in the sulfated waste cotton velvet removed earlier, in 1 weight portion sulfated waste cotton velvet: the ratio water intaking of 15 weight parts waters, detect the resulting amount that should add alkali by metering and add NaOH in proportion, stir and fully dissolving, add sulfated waste cotton velvet fully stir in and 6 hours, filter and dry with aperture 75 μ m sieve then to moisture and be lower than 30%, it is 8% liquor natrii hypochloritis's solution that velveteen after the neutralization is immersed concentration expressed in percentage by weight, soaked 3 hours, filter and dry with aperture 75 μ m sieve then to moisture and be lower than 30%, extremely neutral with the clear water washing, pH value is between 6.8～7.2, insert under 115 ℃ of steam and dry, pulverized the sieve in 150 μ m apertures to moisture≤8%.
Embodiment 4:
The sulfated waste cotton velvet of getting 1Kg immerses in the 12Kg water and fully stirred 20 minutes, quantitatively add sodium carbonate several times, add for the first time 50g, add 20g afterwards at every turn, all stirred 30 minutes after each the adding, test is each to add the acidity of mixed liquor behind the alkali, up to ph value of mixture greater than 7, get that time, write down the ratio that every Kg water should add the amount of alkali near 7; With the 2mm sieve big the mixing in the sulfated waste cotton velvet removed earlier, in 1 weight portion sulfated waste cotton velvet: the ratio water intaking of 12 weight parts waters, detect the resulting amount that should add alkali by metering and add sodium carbonate in proportion, stir and fully dissolving, add sulfated waste cotton velvet fully stir in and 7 hours, filter and dry with aperture 75 μ m sieve then to moisture and be lower than 30%, immerse and be heated to 60 ℃ of slow stirrings 4 hours in weight percent concentration 3% sodium hydroxide solution, filter and dry to moisture with aperture 75 μ m sieve and be lower than 30%, immerse 3% sodium carbonate liquor again and be heated to 60 ℃ of slow stirrings 4 hours, filter and dry to moisture with aperture 75 μ m sieve and be lower than 30%, liquor natrii hypochloritis with weight percent concentration 8% soaked 7 hours down for 60 ℃ in temperature afterwards, filter and dry to moisture with aperture 75 μ m sieve and be lower than 20%, extremely neutral with the clear water washing, pH value is between 6.9～7.2, insert under 120 ℃ of steam and dry, pulverized the sieve in 180 μ m apertures to moisture≤7%.
Embodiment 5:
The sulfated waste cotton velvet of getting 1Kg immerses in the 6Kg water and fully stirred 20 minutes, quantitatively add sodium carbonate several times, add for the first time 50g, add 10g afterwards at every turn, all stirred 30 minutes after each the adding, test is each to add the acidity of mixed liquor behind the alkali, up to ph value of mixture greater than 7, get that time, write down the ratio that every Kg water should add the amount of alkali near 7; With the 2mm sieve big the mixing in the sulfated waste cotton velvet removed earlier, in 1 weight portion sulfated waste cotton velvet: the ratio water intaking of 6 weight parts waters, detect the resulting amount that should add alkali by metering and add sodium carbonate in proportion, stir and fully dissolving, add sulfated waste cotton velvet fully stir in and 4 hours, filter and dry with aperture 75 μ m sieve then to moisture and be lower than 20%, immersing concentration expressed in percentage by weight is 10% clorox, soaked 5 hours in the mixed solution of sodium chloride, clorox, sodium chloride is pressed arbitrary proportion and is mixed, filter and dry to moisture with aperture 75 μ m sieve and be lower than 20%, extremely neutral with the clear water washing, pH value is between 6.8～7.3, insert under 115 ℃ of steam and dry, pulverized the sieve in 125 μ m apertures to moisture≤8%.
Embodiment 6:
The sulfated waste cotton velvet of getting 1Kg immerses in the 10Kg water and fully stirred 25 minutes, quantitatively add calcium hydroxide several times, add for the first time 30g, add 20g afterwards at every turn, all stirred 20 minutes after each the adding, test is each to add the acidity of mixed liquor behind the alkali, up to ph value of mixture greater than 7, get that time, write down the ratio that every Kg water should add the amount of alkali near 7; With the 2.5mm sieve big the mixing in the sulfated waste cotton velvet removed earlier, in 1 weight portion sulfated waste cotton velvet: the ratio water intaking of 10 weight parts waters, detect the resulting amount that should add alkali by metering and add calcium hydroxide in proportion, stir and fully dissolving, add sulfated waste cotton velvet fully stir in and 5 hours, filter and dry with aperture 100 μ m sieve then to moisture and be lower than 20%, immerse concentration expressed in percentage by weight and be among 8% the liquor natrii hypochloritis and soaked 4 hours, filter and dry to moisture with aperture 100 μ m sieve and be lower than 20%, extremely neutral with the clear water washing, pH value is between 6.8～7.3, insert under 115 ℃ of steam and dry, pulverized the sieve in 180 μ m apertures to moisture≤5%.
Embodiment 7:
The sulfated waste cotton velvet of getting 1Kg immerses in the 7Kg water and fully stirred 30 minutes, quantitatively add NaOH several times, add 30g at every turn, adding the back stirred 30 minutes, the acidity of mixed liquor behind the each adding of the test alkali, greater than 7, get that time up to ph value of mixture, write down the ratio that every Kg water should add the amount of alkali near 7; With the 4mm sieve big the mixing in the sulfated waste cotton velvet removed earlier, in 1 weight portion sulfated waste cotton velvet: the ratio water intaking of 5 weight parts waters, detect the resulting amount that should add alkali by metering and add NaOH in proportion, stir and fully dissolving, add sulfated waste cotton velvet fully stir in and 2.5 hours, filter and dry with aperture 100 μ m sieve then to moisture and be lower than 25%, being heated to 55 ℃ in the sodium hydroxide solution of immersion weight percent concentration 2% slowly stirred 6 hours, filter and dry to moisture with aperture 125 μ m sieve and be lower than 30%, immerse 2% sodium carbonate liquor again and be heated to 55 ℃ of slow stirrings 5 hours, filter and dry to moisture with aperture 100 μ m sieve and be lower than 30%, liquor natrii hypochloritis with weight percent concentration 5% soaked 5 hours down for 55 ℃ in temperature afterwards, filter and dry to moisture with aperture 75 μ m sieve and be lower than 20%, extremely neutral with the clear water washing, pH value is between 6.9～7.1, insert under 118 ℃ of steam and dry, pulverized the sieve in 180 μ m apertures to moisture≤7%.
Embodiment 8:
The sulfated waste cotton velvet of getting 1Kg immerses in the 8Kg water and fully stirred 30 minutes, quantitatively add NaOH several times, add for the first time 30g, add 10g afterwards at every turn, add the back and stirred 30 minutes, test is each to add the acidity of mixed liquor behind the alkali, up to ph value of mixture greater than 7, get that time, write down the ratio that every Kg water should add the amount of alkali near 7; With the 2mm sieve big the mixing in the sulfated waste cotton velvet removed earlier, in 1 weight portion sulfated waste cotton velvet: the ratio water intaking of 8 weight parts waters, detect the resulting amount that should add alkali by metering and add NaOH in proportion, stir and fully dissolving, add sulfated waste cotton velvet fully stir in and 1.5 hours, filter and dry with aperture 90 μ m sieve then to moisture and be lower than 25%, being heated to 65 ℃ in the sodium hydroxide solution of immersion weight percent concentration 1.5% slowly stirred 4 hours, filter and dry to moisture with aperture 125 μ m sieve and be lower than 30%, immerse 2% sodium carbonate liquor again and be heated to 65 ℃ of slow stirrings 4 hours, filter and dry to moisture with aperture 90 μ m sieve and be lower than 30%, liquor natrii hypochloritis with weight percent concentration 5% soaked 6 hours down for 55 ℃ in temperature afterwards, filter and dry to moisture with aperture 75 μ m sieve and be lower than 20%, extremely neutral with the clear water washing, pH value is between 6.8～7.2, insert under 112 ℃ of steam and dry, pulverized the sieve in 180 μ m apertures to moisture≤7%.
Embodiment 9:
The sulfated waste cotton velvet of getting 1Kg immerses in the 15Kg water and fully stirred 15 minutes, quantitatively add NaOH several times, add for the first time 40g, for the second time add 30g, add 10g afterwards at every turn, all stirred 50 minutes after each the adding, the acidity of mixed liquor behind the each adding of the test alkali, greater than 7, get that time up to ph value of mixture, write down the ratio that every Kg water should add the amount of alkali near 7; With the 2mm sieve big the mixing in the sulfated waste cotton velvet removed earlier, in 1 weight portion sulfated waste cotton velvet: the ratio water intaking of 15 weight parts waters, detect the resulting amount that should add alkali by metering and add NaOH in proportion, stir and fully dissolving, add sulfated waste cotton velvet fully stir in and 5.5 hours, filter and dry with aperture 100 μ m sieve then to moisture and be lower than 30%, it is 8% liquor natrii hypochloritis's solution that velveteen after the neutralization is immersed concentration expressed in percentage by weight, soaked 3 hours, filter and dry with aperture 75 μ m sieve then to moisture and be lower than 30%, extremely neutral with the clear water washing, pH value is between 6.7～7.5, insert under 115 ℃ of steam and dry, pulverized the sieve in 105 μ m apertures to moisture≤6%.
Claims (3)
1. use the technology for producing microcrystalline cellulose with sulfated waste cotton velvet method for one kind, mainly be made up of following technical process: metering detection, quantitatively neutralization, bleaching, cleaning, oven dry, crushing screening operation is characterized in that:
Described metering detects: the sulfated waste cotton velvet of getting a weight portion immerses in 5～15 weight parts waters and fully stirred 15～30 minutes, quantitatively also add alkali at least at twice: one or both in NaOH, sodium carbonate, the calcium hydroxide, and the acidity of test mixing liquid at any time, up to the pH of mixed value is 5～10, writes down the amount that every weight parts water should add alkali;
Described quantitatively in and operation be: get 5～15 weight parts waters by 1 weight portion sulfated waste cotton velvet, detect in the alkali that the resulting amount that should add alkali adds metering checkout program in proportion one or both by metering, stir and fully dissolving, during fully stirring, the adding sulfated waste cotton velvet, enters bleaching process after filtering then and drying with 1～7 hour;
Described bleaching process is: successively immerse in weight percent concentration 1～3% sodium hydroxide solution and 1～3% sodium carbonate liquor and be heated to 60～80 ℃ each 3～10 hours, soaked 5～7 hours down for 45～60 ℃ in temperature with the liquor natrii hypochloritis of weight percent concentration 1～3% afterwards;
Described baking operation is a steaming process.
2. the technology for producing microcrystalline cellulose with sulfated waste cotton velvet method of using according to claim 1, it is characterized in that described metering detects and quantitatively in and the pH value described in the operation be 7～8.
3. the technology for producing microcrystalline cellulose with sulfated waste cotton velvet method of using according to claim 1 and 2 is characterized in that in the process of the quantitative adding alkali that described metering detects, and the alkali number that adds test after reaching for the second time is than reducing one by one the first time.
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| CN2008100729533A CN101368347B (en) | 2008-09-12 | 2008-09-12 | Technique for producing mlcrocrystalline cellulose by sulfated waste velveteen |
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| CN101368347B true CN101368347B (en) | 2010-12-15 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102747635A (en) * | 2012-07-13 | 2012-10-24 | 钱军 | Method for producing microcrystalline cellulose through sulfated waste cotton velvet |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101551317B (en) * | 2009-05-14 | 2011-03-30 | 宜宾海丝特纤维有限责任公司 | Measuring method for viscosity of alkali cellulose |
| CN102286892A (en) * | 2011-09-05 | 2011-12-21 | 安徽山河药用辅料股份有限公司 | Preparation method of microcrystalline cellulose for food thickening agents |
| CN103122592B (en) * | 2011-11-18 | 2015-01-07 | 奎屯新大陆化学有限公司 | Method for preparing microcrystalline cellulose from waste cotton |
| CN102587182A (en) * | 2012-02-04 | 2012-07-18 | 安徽山河药用辅料股份有限公司 | Preparation method of microcrystalline cellulose for toothpaste |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1081185A (en) * | 1992-07-04 | 1994-01-26 | 苏志刚 | Use technology for producing microcrystalline cellulose with sulfated waste cotton velvet |
| CN101067287A (en) * | 2007-05-31 | 2007-11-07 | 王光建 | Producing technology for microcrystalline cellulose with waste acid cotton linter |
-
2008
- 2008-09-12 CN CN2008100729533A patent/CN101368347B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1081185A (en) * | 1992-07-04 | 1994-01-26 | 苏志刚 | Use technology for producing microcrystalline cellulose with sulfated waste cotton velvet |
| CN101067287A (en) * | 2007-05-31 | 2007-11-07 | 王光建 | Producing technology for microcrystalline cellulose with waste acid cotton linter |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102747635A (en) * | 2012-07-13 | 2012-10-24 | 钱军 | Method for producing microcrystalline cellulose through sulfated waste cotton velvet |
| CN102747635B (en) * | 2012-07-13 | 2015-02-18 | 钱军 | Method for producing microcrystalline cellulose through sulfated waste cotton velvet |
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| CN101368347A (en) | 2009-02-18 |
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