CN100443504C - Method of extracting pectin from waste liquor of white paper mulberry bast pulping - Google Patents
Method of extracting pectin from waste liquor of white paper mulberry bast pulping Download PDFInfo
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- CN100443504C CN100443504C CNB2006101046510A CN200610104651A CN100443504C CN 100443504 C CN100443504 C CN 100443504C CN B2006101046510 A CNB2006101046510 A CN B2006101046510A CN 200610104651 A CN200610104651 A CN 200610104651A CN 100443504 C CN100443504 C CN 100443504C
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Abstract
The process of extracting pectin from waste boiling liquid from pulping paper-mulberry bark includes the following steps: adding saturated Al2(SO4)3 solution to the waste boiling liquid while stirring to precipitate pectin; separating pectin-aluminum precipitate from the solution, vacuum suction filtering to obtain pectin-aluminum precipitate; rinsing the pectin-aluminum precipitate with desalting solution and vacuum suction filtering to separate out pectin precipitate; rinsing the pectin precipitate with alcohol and vacuum drying to obtain pectin product. The waste boiling liquid with pectin extracted has greatly lowered BOD, COD and chroma and easy post-treatment.
Description
Technical field
The present invention relates to a kind of extracting pectin, particularly a kind of method of from waste liquor of white paper mulberry bast pulping, extracting pectin.
Background technology
White structure skin peroxide oxalate cooking waste liquor is to be the boiling chemical with oxalate, hydrogen peroxide and sodium hydroxide, dialogue structure skin carries out the waste liquid that produces in the pulping process treating processes, this waste liquid contains the degradation product of remaining boiling chemical, pectin, lignin and carbohydrate, and color is a brown.
Because white structure hide fiber material chemical component and structural singularity, the key of its slurrying is a bonded pectin substance between de-fibering, and next is only delignification.White structure skin peroxide oxalate pulping process just is based on this characteristics generation.Oxalate is good pectolytic mediator, can remove pectin effectively under certain condition, makes interfibrous combination become loose, thereby isolates single fiber.Because the oxalate pulping process provides possibility for producing high whiteness, high yield, high-quality structure hide fiber paper pulp, become the important method of present structure leather slurry.
The maximum characteristics of white structure skin peroxide oxalate slurrying are exactly that steam economy is few, pectin removal efficiency height, paper pulp yield and pulp brightness height, on a small scale white structure leather slurry papermaking enterprise provide a kind of relative cost lower, pollute few pulping process.The general scale of enterprises in pulp and paper industry that present China is raw material with the phloem fiber is less, and adopts the one-time investment of chemical in the combustion method recovery waste liquid too big, and enterprise generally is difficult to bear.And in the white structure skin peroxide oxalate boiling, alkali charge is original just very low, and it is infeasible therefore adopting the combustion method alkali recovery technology.Be dissolved with a large amount of pectin in the white structure skin peroxide oxalate cooking waste liquor, and pectin has good pectisation, make cooking waste liquor viscosity higher, and along with the reduction of laying temperature and the prolongation of time, it is as a form of gel that waste liquid can become, this moment mobile extreme difference, this brings great difficulty to subsequent wastewater treatment.So there is very big difficulty in the processing of at present white structure skin peroxide oxalate cooking waste liquor.
Pectin has the effect of good gelling and stable emulsifying, has a wide range of applications in foodstuffs industry, medicine industry, light industry.Pectin is as a kind of important additive, and according to reports, the present annual requirement in the whole world and rises with annual about 5% speed more than 16000t.
If the unprocessed just directly discharging of waste liquid not only can cause the serious environmental pollution, and can waste a large amount of useful matter pectin, this is not meet the comprehensive utilization of resource and environment protection theory.There is very big difficulty in the processing of at present white structure skin peroxide oxalate cooking waste liquor, and the method for also effectively not handling about structure skin peroxide oxalate cooking waste liquor at present.
Summary of the invention
The objective of the invention is to overcome the shortcoming of above-mentioned prior art, provide a kind of extraction process simply from waste liquor of white paper mulberry bast pulping, to extract the method for pectin.It has not only alleviated the pollution of environment, and can turn waste into wealth.
For achieving the above object, the technical solution used in the present invention is: at first get 100 parts of white structure skin peroxide oxalate cooking waste liquors, continue to stir and add gradually 8～12 parts of saturated Al
2(SO
4)
3Solution makes pectin be converted into pectin aluminium and precipitates fully; Be placed on 40 ℃～70 ℃ insulations then and leave standstill 50min～80min, the pectin aluminum precipitation is separated out from solution, suction filtration under the vacuum condition is isolated the pectin aluminum precipitation; With isolated pectin aluminum precipitation with 80～110 parts of demineralised liquid rinsings after, vacuum filtration is isolated pectin precipitation; Said demineralised liquid is to be got by 60: 1～4: 36～39 volume ratio is mixed by dehydrated alcohol, 98% vitriol oil and water; Be the isolating pectin precipitation of 50%～70% alcohol rinsing with volumetric concentration again, and then under 60 ℃ of vacuum, be drying to obtain the pectin finished product.
Adopt extracting method of the present invention to extract that BOD, the COD of cooking waste liquor reduces significantly behind the pectin, respectively only for extracting 27.8% and 26.7% before the pectin, also less than original 1/3rd, pollution load reduces colourity significantly.And can gel after the waste liquid cooling, good fluidity, for subsequent wastewater treatment provides may.
Embodiment
Embodiment 1, at first gets 100 parts of white structure skin peroxide oxalate cooking waste liquors, continues to stir and add gradually 12 parts of saturated Al
2(SO
4)
3Solution precipitates pectin fully; Be placed on 40 ℃ of insulations then and leave standstill 60min, the pectin aluminum precipitation is separated out from solution, suction filtration under the vacuum condition is isolated the pectin aluminum precipitation; With isolated pectin aluminum precipitation with 80 parts of demineralised liquid rinsings after, vacuum filtration is isolated pectin precipitation; Said demineralised liquid is to be got by 60: 1: 38 volume ratio is mixed by dehydrated alcohol, 98% vitriol oil and water; Be the isolating pectin precipitation of 70% alcohol rinsing with volumetric concentration again, and then under 60 ℃ of vacuum, be drying to obtain the pectin finished product.
Embodiment 2, at first get 100 parts of white structure skin peroxide oxalate cooking waste liquors, continue to stir and add gradually 10 parts of saturated Al
2(SO
4)
3Solution precipitates pectin fully; Be placed on 60 ℃ of insulations then and leave standstill 80min, the pectin aluminum precipitation is separated out from solution, suction filtration under the vacuum condition is isolated the pectin aluminum precipitation; With isolated pectin aluminum precipitation with 100 parts of demineralised liquid rinsings after, vacuum filtration is isolated pectin precipitation; Said demineralised liquid is to be got by 60: 3: 36 volume ratio is mixed by dehydrated alcohol, 98% vitriol oil and water; Be the isolating pectin precipitation of 50% alcohol rinsing with volumetric concentration again, and then under 60 ℃ of vacuum, be drying to obtain the pectin finished product.
Embodiment 3, at first get 100 parts of white structure skin peroxide oxalate cooking waste liquors, continue to stir and add gradually 8 parts of saturated Al
2(SO
4)
3Solution precipitates pectin fully; Be placed on 70 ℃ of insulations then and leave standstill 50min, the pectin aluminum precipitation is separated out from solution, suction filtration under the vacuum condition is isolated the pectin aluminum precipitation; With isolated pectin aluminum precipitation with 90 parts of demineralised liquid rinsings after, vacuum filtration is isolated pectin precipitation; Said demineralised liquid is to be got by 60: 2: 39 volume ratio is mixed by dehydrated alcohol, 98% vitriol oil and water; Be the isolating pectin precipitation of 60% alcohol rinsing with volumetric concentration again, and then under 60 ℃ of vacuum, be drying to obtain the pectin finished product.
Embodiment 4, at first get 100 parts of white structure skin peroxide oxalate cooking waste liquors, continue to stir and add gradually 11 parts of saturated Al
2(SO
4)
3Solution precipitates pectin fully; Be placed on 50 ℃ of insulations then and leave standstill 70min, the pectin aluminum precipitation is separated out from solution, suction filtration under the vacuum condition is isolated the pectin aluminum precipitation; With isolated pectin aluminum precipitation with 110 parts of demineralised liquid rinsings after, vacuum filtration is isolated pectin precipitation; Said demineralised liquid is to be got by 60: 4: 37 volume ratio is mixed by dehydrated alcohol, 98% vitriol oil and water; Be the isolating pectin precipitation of 55% alcohol rinsing with volumetric concentration again, and then under 60 ℃ of vacuum, be drying to obtain the pectin finished product.
Embodiment 5, at first get 100 parts of white structure skin peroxide oxalate cooking waste liquors, continue to stir and add gradually 9 parts of saturated Al
2(SO
4)
3Solution precipitates pectin fully; Be placed on 62 ℃ of insulations then and leave standstill 56min, the pectin aluminum precipitation is separated out from solution, suction filtration under the vacuum condition is isolated the pectin aluminum precipitation; With isolated pectin aluminum precipitation with 95 parts of demineralised liquid rinsings after, vacuum filtration is isolated pectin precipitation; Said demineralised liquid is to be got by 60: 2: 36 volume ratio is mixed by dehydrated alcohol, 98% vitriol oil and water; Be the isolating pectin precipitation of 65% alcohol rinsing with volumetric concentration again, and then under 60 ℃ of vacuum, be drying to obtain the pectin finished product.
Claims (6)
1, a kind of method of extracting pectin from waste liquor of white paper mulberry bast pulping is characterized in that:
1) at first gets 100 parts of white structure skin peroxide oxalate cooking waste liquors, continue to stir and add gradually 8～12 parts of saturated Al
2(SO
4)
3Solution makes pectin be converted into pectin aluminium and precipitates fully;
2) be placed on 40 ℃～70 ℃ insulations then and leave standstill 50min～80min, the pectin aluminum precipitation is separated out from solution, suction filtration under the vacuum condition is isolated the pectin aluminum precipitation;
3) with isolated pectin aluminum precipitation with 80～110 parts of demineralised liquid rinsings after, vacuum filtration is isolated pectin precipitation; Said demineralised liquid is to be got by 60: 1～4: 36～39 volume ratio is mixed by dehydrated alcohol, 98% vitriol oil and water;
4) be the isolating pectin precipitation of 50%～70% alcohol rinsing with volumetric concentration again, and then under 60 ℃ of vacuum, be drying to obtain the pectin finished product.
2, the method for extracting pectin from waste liquor of white paper mulberry bast pulping according to claim 1 is characterized in that: at first get 100 parts of white structure skin peroxide oxalate cooking waste liquors, continue to stir and add gradually 12 parts of saturated Al
2(SO
4)
3Solution makes pectin be converted into pectin aluminium and precipitates fully; Be placed on 40 ℃ of insulations then and leave standstill 60min, the pectin aluminum precipitation is separated out from solution, suction filtration under the vacuum condition is isolated the pectin aluminum precipitation; With isolated pectin aluminum precipitation with 80 parts of demineralised liquid rinsings after, vacuum filtration is isolated pectin precipitation; Said demineralised liquid is to be got by 60: 1: 38 volume ratio is mixed by dehydrated alcohol, 98% vitriol oil and water; Be the isolating pectin precipitation of 70% alcohol rinsing with volumetric concentration again, and then under 60 ℃ of vacuum, be drying to obtain the pectin finished product.
3, the method for extracting pectin from waste liquor of white paper mulberry bast pulping according to claim 1 is characterized in that: at first get 100 parts of white structure skin peroxide oxalate cooking waste liquors, continue to stir and add gradually 10 parts of saturated Al
2(SO
4)
3Solution makes pectin be converted into pectin aluminium and precipitates fully; Be placed on 60 ℃ of insulations then and leave standstill 80min, the pectin aluminum precipitation is separated out from solution, suction filtration under the vacuum condition is isolated the pectin aluminum precipitation; With isolated pectin aluminum precipitation with 100 parts of demineralised liquid rinsings after, vacuum filtration is isolated pectin precipitation; Said demineralised liquid is to be got by 60: 3: 36 volume ratio is mixed by dehydrated alcohol, 98% vitriol oil and water; Be the isolating pectin precipitation of 50% alcohol rinsing with volumetric concentration again, and then under 60 ℃ of vacuum, be drying to obtain the pectin finished product.
4, the method for extracting pectin from waste liquor of white paper mulberry bast pulping according to claim 1 is characterized in that: at first get 100 parts of white structure skin peroxide oxalate cooking waste liquors, continue to stir and add gradually 8 parts of saturated Al
2(SO
4)
3Solution makes pectin be converted into pectin aluminium and precipitates fully; Be placed on 70 ℃ of insulations then and leave standstill 50min, the pectin aluminum precipitation is separated out from solution, suction filtration under the vacuum condition is isolated the pectin aluminum precipitation; With isolated pectin aluminum precipitation with 90 parts of demineralised liquid rinsings after, vacuum filtration is isolated pectin precipitation; Said demineralised liquid is to be got by 60: 2: 39 volume ratio is mixed by dehydrated alcohol, 98% vitriol oil and water; Be the isolating pectin precipitation of 60% alcohol rinsing with volumetric concentration again, and then under 60 ℃ of vacuum, be drying to obtain the pectin finished product.
5, the method for extracting pectin from waste liquor of white paper mulberry bast pulping according to claim 1 is characterized in that: at first get 100 parts of white structure skin peroxide oxalate cooking waste liquors, continue to stir and add gradually 11 parts of saturated Al
2(SO
4)
3Solution makes pectin be converted into pectin aluminium and precipitates fully; Be placed on 50 ℃ of insulations then and leave standstill 70min, the pectin aluminum precipitation is separated out from solution, suction filtration under the vacuum condition is isolated the pectin aluminum precipitation; With isolated pectin aluminum precipitation with 110 parts of demineralised liquid rinsings after, vacuum filtration is isolated pectin precipitation; Said demineralised liquid is to be got by 60: 4: 37 volume ratio is mixed by dehydrated alcohol, 98% vitriol oil and water; Be the isolating pectin precipitation of 55% alcohol rinsing with volumetric concentration again, and then under 60 ℃ of vacuum, be drying to obtain the pectin finished product.
6, the method for extracting pectin from waste liquor of white paper mulberry bast pulping according to claim 1 is characterized in that: at first get 100 parts of white structure skin peroxide oxalate cooking waste liquors, continue to stir and add gradually 9 parts of saturated Al
2(SO
4)
3Solution makes pectin be converted into pectin aluminium and precipitates fully; Be placed on 62 ℃ of insulations then and leave standstill 56min, the pectin aluminum precipitation is separated out from solution, suction filtration under the vacuum condition is isolated the pectin aluminum precipitation; With isolated pectin aluminum precipitation with 95 parts of demineralised liquid rinsings after, vacuum filtration is isolated pectin precipitation; Said demineralised liquid is to be got by 60: 2: 36 volume ratio is mixed by dehydrated alcohol, 98% vitriol oil and water; Be the isolating pectin precipitation of 65% alcohol rinsing with volumetric concentration again, and then under 60 ℃ of vacuum, be drying to obtain the pectin finished product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101046510A CN100443504C (en) | 2006-09-26 | 2006-09-26 | Method of extracting pectin from waste liquor of white paper mulberry bast pulping |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101046510A CN100443504C (en) | 2006-09-26 | 2006-09-26 | Method of extracting pectin from waste liquor of white paper mulberry bast pulping |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1927891A CN1927891A (en) | 2007-03-14 |
| CN100443504C true CN100443504C (en) | 2008-12-17 |
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|---|---|---|---|
| CNB2006101046510A Expired - Fee Related CN100443504C (en) | 2006-09-26 | 2006-09-26 | Method of extracting pectin from waste liquor of white paper mulberry bast pulping |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1055466A (en) * | 1990-04-07 | 1991-10-23 | 中国科学院科理高技术公司成都分公司 | A kind of slaine method is obtained through refining the method for pectin |
| CN1107858A (en) * | 1994-10-06 | 1995-09-06 | 西南农业大学 | Method for extracting pectin from lemon peel |
| CN1442431A (en) * | 2003-04-02 | 2003-09-17 | 石启田 | Ginkgo pectin extracted by using ginkgo external seed peel as raw material and extraction method |
| CN1526738A (en) * | 2003-09-23 | 2004-09-08 | 武汉化工学院 | Method of preparing pectin with orange peel |
-
2006
- 2006-09-26 CN CNB2006101046510A patent/CN100443504C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1055466A (en) * | 1990-04-07 | 1991-10-23 | 中国科学院科理高技术公司成都分公司 | A kind of slaine method is obtained through refining the method for pectin |
| CN1107858A (en) * | 1994-10-06 | 1995-09-06 | 西南农业大学 | Method for extracting pectin from lemon peel |
| CN1442431A (en) * | 2003-04-02 | 2003-09-17 | 石启田 | Ginkgo pectin extracted by using ginkgo external seed peel as raw material and extraction method |
| CN1526738A (en) * | 2003-09-23 | 2004-09-08 | 武汉化工学院 | Method of preparing pectin with orange peel |
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|---|---|
| CN1927891A (en) | 2007-03-14 |
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Granted publication date: 20081217 Termination date: 20110926 |