CN101649570B - A low-pollution preparation process of wheat straw cellulose - Google Patents
A low-pollution preparation process of wheat straw cellulose Download PDFInfo
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- CN101649570B CN101649570B CN2009100237675A CN200910023767A CN101649570B CN 101649570 B CN101649570 B CN 101649570B CN 2009100237675 A CN2009100237675 A CN 2009100237675A CN 200910023767 A CN200910023767 A CN 200910023767A CN 101649570 B CN101649570 B CN 101649570B
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Abstract
The invention relates to a process for preparing wheatgrass cellulose with low pollution. The process comprises the following steps: putting wheatgrass into an ethanol water solution, dissolving most of lignin and hemicellulose in the wheatgrass at high temperature, then dispersing the wheatgrass into water, adding MgSO4, introducing oxygen, filtering after further removing the lignin and part ofthe hemicellulose under a heating condition, washing a cellulose crude product, introducing ozone, removing the residual lignin and the residual hemicellulose to obtain a cellulose product; finally, filtering, washing the cellulose product, adding alkali, regulating the pH value to 8-12, adding H2O2, carrying out heat processing, filtering, washing to obtain a pure cellulose product after being refined. The invention adopts a low-pollution ethanol method to decompose the raw material of the wheatgrass, separates and refines the cellulose in the wheatgrass by a process adopting pollution-free chemical reagents, such as the oxygen, the ozone, the H2O2 and the like, to carry out subsequent processing, relieves the emergent shortage problem of common cellulose resources, such as wood, cotton and the like, and also makes full use of the agricultural waste of wheat straw resource.
Description
Technical field
The invention belongs to the natural polymer technical field, be specifically related to a kind of low pollution preparation technology of wheatgrass cellulose.
Background technology
Cellulose is the main raw material of preparation microcrystalline cellulose, and the natural polymer product that microcrystalline cellulose is made up of free flowable cellulose crystal is widely used in every field.As be used in excipients in the medicine, emulsion in the food industry and foaming stabiliser etc., paste in the light industry and emulsus cosmetic additive agent etc.Usually, the raw cellulose of preparation microcrystalline cellulose is to be that raw material prepares by series of processes such as alkaline cooking slurrying, bleachings with timber and cotton, its production technology has very big shortcoming: the one, and cotton is relative in short supply with resources such as timber, has limited the production scale of high purity cellulose and microcrystalline cellulose thereof; The 2nd, existing cellulose isolation technics adopts caustic soda boiling and chlorine bleach technology more, and its waste liquid environmental pollution is big.
Summary of the invention
The object of the present invention is to provide a kind of preparation technology simple, separation and subtractive process do not have the low pollution preparation technology that chlorine does not have sulphur and do not have the wheatgrass cellulose of a large amount of caustic soda uses.
For achieving the above object, the technical solution used in the present invention is:
1) at first, by solid-to-liquid ratio is that wheat straw to be placed volumetric concentration in 1: 3～1: 12 be 10%～80% ethanol water, handle 30～120min down at 80～200 ℃, make most of lignin and hemicellulose in the dissolve with ethanol solution wheat straw, obtain coarse product of cellulose;
2) secondly, coarse product of cellulose is dispersed in the water, the coarse product of cellulose of adding account for water quality 3%～25%, regulating pH value then is 8～13, and the MgSO of adding coarse product of cellulose quality 0.1%～1.6%
4As protective agent, be 0.2～1.2MPa at oxygen pressure, temperature is 50～130 ℃ and handles 20～120min down, further removes lignin and part hemicellulose;
3) then, filter and coarse product of cellulose is washed, adding the second acid for adjusting pH value in the coarse product of cellulose after washing is 2～5, adding the mass concentration that entry makes coarse product of cellulose again is 10%～50%, at normal temperatures, feed the ozone of coarse product of cellulose quality 0.2%～3%, processing 20～90min removes residual lignin and hemicellulose obtains cellulose products;
4) last, filter and the plain product of washing the fibre, regulating its mass concentration is 2%～30%, adding alkali adjusting pH value then is 8～12, and adds the H of cellulose products quality 3%～15%
2O
2, under 40～110 ℃ of temperature, handle 30～120min, washing promptly obtains the pure cellulose products in refining back.
The present invention adopts low pollution ethanol method to decompose wheat straw raw material, adopts oxygen, ozone, H
2O
2The technology of carrying out subsequent treatment etc. pollution-free chemical reagent is separated the cellulose in the wheat straw and is made with extra care, and this separation and process for refining environmental pollution are minimum, therefore has very high environment protection significance.In addition, adopt wheat stalk, both alleviated the problem in short supply of cellulose resource commonly used such as timber, cotton, made full use of the agricultural wastes wheat straw resource again, and turned waste into wealth, produce very big economic benefit and social benefit as raw material.
The specific embodiment
Embodiment 1:
1) at first, be that wheat straw to be placed volumetric concentration in 1: 3 be 50% ethanol water by solid-to-liquid ratio, handle 120min down at 80 ℃, make most of lignin and hemicellulose in the dissolve with ethanol solution wheat straw, obtain coarse product of cellulose;
2) secondly, coarse product of cellulose is dispersed in the water, the coarse product of cellulose of adding account for water quality 10%, regulating pH value then is 8, and the MgSO of adding coarse product of cellulose quality 0.5%
4As protective agent, be 1.0MPa at oxygen pressure, temperature is 130 ℃ and handles 120min down, further removes lignin and part hemicellulose;
3) then, filter and coarse product of cellulose is washed, adding the second acid for adjusting pH value in the coarse product of cellulose after washing is 4, adding the mass concentration that entry makes coarse product of cellulose again is 20%, at normal temperatures, feed the ozone of coarse product of cellulose quality 0.2%, processing 50min removes residual lignin and hemicellulose obtains cellulose products;
4) last, filter and the plain product of washing the fibre, regulating its mass concentration is 15%, adding alkali adjusting pH value then is 10, and adds the H of cellulose products quality 15%
2O
2, under 40 ℃ of temperature, handle 120min, washing promptly obtains the pure cellulose products in refining back.
Embodiment 2:
1) at first, be that wheat straw to be placed volumetric concentration in 1: 8 be 30% ethanol water by solid-to-liquid ratio, handle 100min down at 120 ℃, make most of lignin and hemicellulose in the dissolve with ethanol solution wheat straw, obtain coarse product of cellulose;
2) secondly, coarse product of cellulose is dispersed in the water, the coarse product of cellulose of adding account for water quality 16%, regulating pH value then is 10, and the MgSO of adding coarse product of cellulose quality 1.2%
4As protective agent, be 0.6MPa at oxygen pressure, temperature is 100 ℃ and handles 90min down, further removes lignin and part hemicellulose;
3) then, filter and coarse product of cellulose is washed, adding the second acid for adjusting pH value in the coarse product of cellulose after washing is 2, adding the mass concentration that entry makes coarse product of cellulose again is 40%, at normal temperatures, feed the ozone of coarse product of cellulose quality 0.8%, processing 70min removes residual lignin and hemicellulose obtains cellulose products;
4) last, filter and the plain product of washing the fibre, regulating its mass concentration is 2%, adding alkali adjusting pH value then is 8, and adds the H of cellulose products quality 6%
2O
2, under 60 ℃ of temperature, handle 100min, washing promptly obtains the pure cellulose products in refining back.
Embodiment 3:
1) at first, be that wheat straw to be placed volumetric concentration in 1: 5 be 80% ethanol water by solid-to-liquid ratio, handle 80min down at 150 ℃, make most of lignin and hemicellulose in the dissolve with ethanol solution wheat straw, obtain coarse product of cellulose;
2) secondly, coarse product of cellulose is dispersed in the water, the coarse product of cellulose of adding account for water quality 25%, regulating pH value then is 13, and the MgSO of adding coarse product of cellulose quality 0.8%
4As protective agent, be 0.2MPa at oxygen pressure, temperature is 80 ℃ and handles 60min down, further removes lignin and part hemicellulose;
3) then, filter and coarse product of cellulose is washed, adding the second acid for adjusting pH value in the coarse product of cellulose after washing is 5, adding the mass concentration that entry makes coarse product of cellulose again is 10%, at normal temperatures, feed the ozone of coarse product of cellulose quality 1.5%, processing 40min removes residual lignin and hemicellulose obtains cellulose products;
4) last, filter and the plain product of washing the fibre, regulating its mass concentration is 25%, adding alkali adjusting pH value then is 12, and adds the H of cellulose products quality 3%
2O
2, under 80 ℃ of temperature, handle 80min, washing promptly obtains the pure cellulose products in refining back.
Embodiment 4:
1) at first, be that wheat straw to be placed volumetric concentration in 1: 10 be 10% ethanol water by solid-to-liquid ratio, handle 50min down at 180 ℃, make most of lignin and hemicellulose in the dissolve with ethanol solution wheat straw, obtain coarse product of cellulose;
2) secondly, coarse product of cellulose is dispersed in the water, the coarse product of cellulose of adding account for water quality 3%, regulating pH value then is 11, and the MgSO of adding coarse product of cellulose quality 0.1%
4As protective agent, be 0.8MPa at oxygen pressure, temperature is 60 ℃ and handles 40min down, further removes lignin and part hemicellulose;
3) then, filter and coarse product of cellulose is washed, adding the second acid for adjusting pH value in the coarse product of cellulose after washing is 3, adding the mass concentration that entry makes coarse product of cellulose again is 50%, at normal temperatures, feed the ozone of coarse product of cellulose quality 2.2%, processing 20min removes residual lignin and hemicellulose obtains cellulose products;
4) last, filter and the plain product of washing the fibre, regulating its mass concentration is 10%, adding alkali adjusting pH value then is 9, and adds the H of cellulose products quality 10%
2O
2, under 95 ℃ of temperature, handle 50min, washing promptly obtains the pure cellulose products in refining back.
Embodiment 5:
1) at first, be that wheat straw to be placed volumetric concentration in 1: 12 be 60% ethanol water by solid-to-liquid ratio, handle 30min down at 200 ℃, make most of lignin and hemicellulose in the dissolve with ethanol solution wheat straw, obtain coarse product of cellulose;
2) secondly, coarse product of cellulose is dispersed in the water, the coarse product of cellulose of adding account for water quality 20%, regulating pH value then is 9, and the MgSO of adding coarse product of cellulose quality 1.6%
4As protective agent, be 1.2MPa at oxygen pressure, temperature is 50 ℃ and handles 20min down, further removes lignin and part hemicellulose;
3) then, filter and coarse product of cellulose is washed, adding the second acid for adjusting pH value in the coarse product of cellulose after washing is 5, adding the mass concentration that entry makes coarse product of cellulose again is 30%, at normal temperatures, feed the ozone of coarse product of cellulose quality 3%, processing 90min removes residual lignin and hemicellulose obtains cellulose products;
4) last, filter and the plain product of washing the fibre, regulating its mass concentration is 30%, adding alkali adjusting pH value then is 11, and adds the H of cellulose products quality 13%
2O
2, under 110 ℃ of temperature, handle 30min, washing promptly obtains the pure cellulose products in refining back.
Claims (1)
1. the preparation technology of a wheatgrass cellulose is characterized in that:
1) at first, by solid-to-liquid ratio is that wheat straw to be placed volumetric concentration in 1: 3～1: 12 be 10%～80% ethanol water, handle 30～120min down at 80～200 ℃, make most of lignin and hemicellulose in the dissolve with ethanol solution wheat straw, obtain coarse product of cellulose;
2) secondly, coarse product of cellulose is dispersed in the water, the coarse product of cellulose of adding account for water quality 3%～25%, regulating pH value then is 8～13, and the MgSO of adding coarse product of cellulose quality 0.1%～1.6%
4As protective agent, be 0.2～1.2MPa at oxygen pressure, temperature is 50～130 ℃ and handles 20～120min down, further removes lignin and part hemicellulose;
3) then, filter and coarse product of cellulose is washed, adding the second acid for adjusting pH value in the coarse product of cellulose after washing is 2～5, adding the mass concentration that entry makes coarse product of cellulose again is 10%～50%, at normal temperatures, feed the ozone of coarse product of cellulose quality 0.2%～3%, processing 20～90min removes residual lignin and hemicellulose obtains cellulose products;
4) last, filter and the plain product of washing the fibre, regulating its mass concentration is 2%～30%, adding alkali adjusting pH value then is 8～12, and adds the H of cellulose products quality 3%～15%
2O
2, under 40～110 ℃ of temperature, handle 30～120min, washing promptly obtains the pure cellulose products in refining back.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2009100237675A CN101649570B (en) | 2009-09-01 | 2009-09-01 | A low-pollution preparation process of wheat straw cellulose |
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| CN2009100237675A CN101649570B (en) | 2009-09-01 | 2009-09-01 | A low-pollution preparation process of wheat straw cellulose |
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| CN101649570A CN101649570A (en) | 2010-02-17 |
| CN101649570B true CN101649570B (en) | 2011-02-09 |
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| JP5822101B2 (en) * | 2010-08-04 | 2015-11-24 | 愛媛県 | Method for producing cellulose solution, method for producing cellulose precipitate, and method for saccharification of cellulose |
| CN102251424A (en) * | 2011-06-25 | 2011-11-23 | 浙江理工大学 | Method for extracting cellulose in one step |
| CN107475466B (en) * | 2017-08-31 | 2020-12-04 | 四川雅华生物有限公司 | Process for preparing xylose by hydrolyzing hemicellulose with ozone acid |
| CN113529495B (en) * | 2021-07-22 | 2023-03-24 | 广西大学 | Preparation method of biomass-based tableware with high water stability |
| CN113580668B (en) * | 2021-07-22 | 2023-05-30 | 广西大学 | Preparation of a self-adhesive and water-stable paper straw |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0105937A1 (en) * | 1982-10-04 | 1984-04-25 | Baron Howard Steven Strouth | Method of manufacturing alcohol from ligno-cellulose material |
| CN1424332A (en) * | 2002-12-10 | 2003-06-18 | 华南理工大学 | Homogeneous chemical modification of hemicellulose of stalks |
| CN1626555A (en) * | 2003-12-12 | 2005-06-15 | 北京有色金属研究总院 | Carboxymethyl cellulose of a kind of haulm and preparation method |
| CN101182361A (en) * | 2007-12-07 | 2008-05-21 | 华南理工大学 | A method for preparing acetylated hemicellulose using iodine catalysis |
-
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0105937A1 (en) * | 1982-10-04 | 1984-04-25 | Baron Howard Steven Strouth | Method of manufacturing alcohol from ligno-cellulose material |
| CN1424332A (en) * | 2002-12-10 | 2003-06-18 | 华南理工大学 | Homogeneous chemical modification of hemicellulose of stalks |
| CN1626555A (en) * | 2003-12-12 | 2005-06-15 | 北京有色金属研究总院 | Carboxymethyl cellulose of a kind of haulm and preparation method |
| CN101182361A (en) * | 2007-12-07 | 2008-05-21 | 华南理工大学 | A method for preparing acetylated hemicellulose using iodine catalysis |
Non-Patent Citations (1)
| Title |
|---|
| JP昭59-48090A 1984.03.19 |
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