CN102643935A - Method for preparing xylose by using squeezed waste alkali liquor in viscose fiber production process - Google Patents
Method for preparing xylose by using squeezed waste alkali liquor in viscose fiber production process Download PDFInfo
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- CN102643935A CN102643935A CN201210104647XA CN201210104647A CN102643935A CN 102643935 A CN102643935 A CN 102643935A CN 201210104647X A CN201210104647X A CN 201210104647XA CN 201210104647 A CN201210104647 A CN 201210104647A CN 102643935 A CN102643935 A CN 102643935A
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- wood sugar
- semicellulose
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- production process
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- SRBFZHDQGSBBOR-IOVATXLUSA-N D-xylopyranose Chemical compound O[C@@H]1COC(O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-IOVATXLUSA-N 0.000 title claims abstract description 110
- 239000003513 alkali Substances 0.000 title claims abstract description 61
- PYMYPHUHKUWMLA-UHFFFAOYSA-N arabinose Natural products OCC(O)C(O)C(O)C=O PYMYPHUHKUWMLA-UHFFFAOYSA-N 0.000 title claims abstract description 55
- SRBFZHDQGSBBOR-UHFFFAOYSA-N beta-D-Pyranose-Lyxose Natural products OC1COC(O)C(O)C1O SRBFZHDQGSBBOR-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 48
- 239000002699 waste material Substances 0.000 title claims abstract description 42
- 229920000297 Rayon Polymers 0.000 title claims abstract description 32
- 230000008569 process Effects 0.000 title abstract description 12
- 238000007380 fibre production Methods 0.000 title abstract 2
- 230000007062 hydrolysis Effects 0.000 claims abstract description 35
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 35
- 238000004519 manufacturing process Methods 0.000 claims abstract description 33
- 238000001035 drying Methods 0.000 claims abstract description 29
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 24
- 229920002488 Hemicellulose Polymers 0.000 claims abstract description 20
- 238000004094 preconcentration Methods 0.000 claims abstract description 20
- 238000002425 crystallisation Methods 0.000 claims abstract description 18
- 230000008025 crystallization Effects 0.000 claims abstract description 18
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- 238000000926 separation method Methods 0.000 claims abstract description 13
- 238000005342 ion exchange Methods 0.000 claims abstract description 11
- 238000000605 extraction Methods 0.000 claims abstract description 8
- 229960003487 xylose Drugs 0.000 claims description 149
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Substances [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 130
- SRBFZHDQGSBBOR-LECHCGJUSA-N alpha-D-xylose Chemical compound O[C@@H]1CO[C@H](O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-LECHCGJUSA-N 0.000 claims description 97
- 239000000243 solution Substances 0.000 claims description 97
- 239000006188 syrup Substances 0.000 claims description 33
- 235000020357 syrup Nutrition 0.000 claims description 33
- 239000000835 fiber Substances 0.000 claims description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 21
- 239000012141 concentrate Substances 0.000 claims description 21
- 238000001914 filtration Methods 0.000 claims description 20
- 239000000047 product Substances 0.000 claims description 20
- 235000008504 concentrate Nutrition 0.000 claims description 19
- 238000005374 membrane filtration Methods 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 238000001704 evaporation Methods 0.000 claims description 18
- 230000008020 evaporation Effects 0.000 claims description 18
- 239000000843 powder Substances 0.000 claims description 18
- 239000003153 chemical reaction reagent Substances 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 16
- 239000012528 membrane Substances 0.000 claims description 14
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 12
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 12
- 239000007864 aqueous solution Substances 0.000 claims description 12
- 230000008021 deposition Effects 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 230000006837 decompression Effects 0.000 claims description 7
- NKWPZUCBCARRDP-UHFFFAOYSA-L calcium bicarbonate Chemical compound [Ca+2].OC([O-])=O.OC([O-])=O NKWPZUCBCARRDP-UHFFFAOYSA-L 0.000 claims description 6
- 229910000020 calcium bicarbonate Inorganic materials 0.000 claims description 6
- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Substances [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 6
- 235000010216 calcium carbonate Nutrition 0.000 claims description 6
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 6
- 239000000920 calcium hydroxide Substances 0.000 claims description 6
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 6
- 235000011116 calcium hydroxide Nutrition 0.000 claims description 6
- 239000000292 calcium oxide Substances 0.000 claims description 6
- 235000012255 calcium oxide Nutrition 0.000 claims description 6
- 230000008030 elimination Effects 0.000 claims description 6
- 238000003379 elimination reaction Methods 0.000 claims description 6
- 238000009434 installation Methods 0.000 claims description 6
- 235000012204 lemonade/lime carbonate Nutrition 0.000 claims description 6
- 238000001471 micro-filtration Methods 0.000 claims description 6
- -1 poly tetrafluoroethylene Polymers 0.000 claims description 6
- 229940058401 polytetrafluoroethylene Drugs 0.000 claims description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 6
- 239000006228 supernatant Substances 0.000 claims description 6
- 239000002351 wastewater Substances 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 238000004042 decolorization Methods 0.000 abstract 1
- 238000004064 recycling Methods 0.000 abstract 1
- 239000002994 raw material Substances 0.000 description 18
- TVXBFESIOXBWNM-UHFFFAOYSA-N Xylitol Natural products OCCC(O)C(O)C(O)CCO TVXBFESIOXBWNM-UHFFFAOYSA-N 0.000 description 10
- 239000002253 acid Substances 0.000 description 10
- HEBKCHPVOIAQTA-UHFFFAOYSA-N meso ribitol Natural products OCC(O)C(O)C(O)CO HEBKCHPVOIAQTA-UHFFFAOYSA-N 0.000 description 10
- 239000011347 resin Substances 0.000 description 10
- 229920005989 resin Polymers 0.000 description 10
- 239000000811 xylitol Substances 0.000 description 10
- 235000010447 xylitol Nutrition 0.000 description 10
- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 description 10
- 229960002675 xylitol Drugs 0.000 description 10
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 9
- 235000017491 Bambusa tulda Nutrition 0.000 description 9
- 241001330002 Bambuseae Species 0.000 description 9
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 9
- 239000011425 bamboo Substances 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 8
- 238000011069 regeneration method Methods 0.000 description 8
- 239000013078 crystal Substances 0.000 description 6
- 238000007599 discharging Methods 0.000 description 6
- 230000008929 regeneration Effects 0.000 description 6
- 239000003292 glue Substances 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 229920002678 cellulose Polymers 0.000 description 4
- 239000001913 cellulose Substances 0.000 description 4
- 238000011010 flushing procedure Methods 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000002203 pretreatment Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 2
- LPQOADBMXVRBNX-UHFFFAOYSA-N ac1ldcw0 Chemical compound Cl.C1CN(C)CCN1C1=C(F)C=C2C(=O)C(C(O)=O)=CN3CCSC1=C32 LPQOADBMXVRBNX-UHFFFAOYSA-N 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 150000001720 carbohydrates Chemical class 0.000 description 2
- 235000014633 carbohydrates Nutrition 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 239000000796 flavoring agent Substances 0.000 description 2
- 235000019634 flavors Nutrition 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 description 2
- 239000008103 glucose Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000007781 pre-processing Methods 0.000 description 2
- 230000002000 scavenging effect Effects 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 241000609240 Ambelania acida Species 0.000 description 1
- 241000193830 Bacillus <bacterium> Species 0.000 description 1
- 229920003043 Cellulose fiber Polymers 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 229920000875 Dissolving pulp Polymers 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 240000004808 Saccharomyces cerevisiae Species 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 102000011759 adducin Human genes 0.000 description 1
- 108010076723 adducin Proteins 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000002154 agricultural waste Substances 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 239000010905 bagasse Substances 0.000 description 1
- 238000004061 bleaching Methods 0.000 description 1
- 239000001175 calcium sulphate Substances 0.000 description 1
- 235000011132 calcium sulphate Nutrition 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- ZOOODBUHSVUZEM-UHFFFAOYSA-N ethoxymethanedithioic acid Chemical compound CCOC(S)=S ZOOODBUHSVUZEM-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 235000003599 food sweetener Nutrition 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 230000036449 good health Effects 0.000 description 1
- 239000010903 husk Substances 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 230000001900 immune effect Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000004627 regenerated cellulose Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 239000010902 straw Substances 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 235000021147 sweet food Nutrition 0.000 description 1
- 239000003765 sweetening agent Substances 0.000 description 1
- 235000012976 tarts Nutrition 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 239000012991 xanthate Substances 0.000 description 1
Landscapes
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention relates to a method for preparing xylose by using squeezed waste alkali liquor in the viscose fiber production process. The xylose finished product is obtained through the working procedures of hemicellulose solution preparation, hemicellulose extraction, hemicellulose hydrolysis, neutralization deacidification, preconcentration, decolorization, ion exchange, conventional concentration, crystallization, separation and drying. By adopting the technical scheme of the invention, harmful substances such as waste alkali, waste water and the like which pollute the environment and are generated in the viscose production process can be thoroughly eliminated, the standard of the whole-flow clean production can be reached, viscose production enterprises can produce the viscose and the xylose simultaneously, the aim of environmental protection is fulfilled, and the waste recycling is also realized.
Description
Technical field
The present invention relates to a kind of method for preparing wood sugar, more particularly, the present invention relates to a kind of the utilization and squeeze the method that waste lye prepares wood sugar in the production process of viscose fiber.
Background technology
Wood sugar is a kind of reductibility carbohydrate, is a component of pentosan, and molecular formula is C
5H
10O
5The wood sugar sugariness is 72% of a sucrose, and is approaching with the glucose sugariness, and local flavor is also similar with glucose, can improve the local flavor and the mouthfeel of sweet food, suppresses peculiar smell.Wood sugar can be hydrogenated reduction and generate Xylitol in the presence of catalyzer, can be used as the raw material of Xylitol, and wood sugar has good food compatibleness, can mix with amino acid to be easy to generate Maillard reaction in the heat-processed, plays the effect of flavouring.It is functional that wood sugar also has good health care, can grow by interior bifidus bacillus and short its of activating human body enteron aisle, improves the micro-ecological environment of human body, improves the immunological competence of body.In recent years, wood sugar is an important chemical material, and industry is used for producing Xylitol, fodder yeast, and in fields such as food, medicine, chemical industry, leather, dyestuffs purposes is widely arranged all.
At present, also do not find the wood sugar of unbound state so far at nature, natural D-wood sugar is present in the plant with the form of polysaccharide, and content is more in the discarded part of agricultural-food such as corn cob, cotton seed hulls, bagasse, rice husk and other straws, seed cot etc.At home and abroad, wood sugar is quite favored as sweetening agent, the demand sharp increase.Current, the production of wood sugar worldwide, is an infant industry, still is in the starting stage in the production of China's wood sugar.
It is 101643795 that State Intellectual Property Office discloses a publication number on February 10th, 2010; Name is called " the bamboo method that is equipped with wood sugar, Xylitol of a kind of usefulness "; This patent of invention discloses the bamboo method that is equipped with wood sugar, Xylitol of a kind of usefulness; Comprise pre-treatment, hydrolysis, decolouring, IX, concentrate and Crystallization Procedure makes wood sugar that wood sugar is produced Xylitol through hydrogenation indirectly, said pretreatment process comprises washing, hot acid pre-treatment and hot water pre-treatment; Said hydrolyzing process is divided into a hydrolysis and secondary hydrolysis.Use bamboo to be feedstock production wood sugar, Xylitol, the hydrolyzed solution of generation is of light color, and transmittance is high, and assorted sugar is few in the hydrolyzed solution, helps later separation and proposes, and the wood sugar quality that obtains is high; It is that the used catalyzer of raw material is compared than other agricultural wastes that wood sugar prepares the used catalyzer of Xylitol through shortening, and catalyst consumption obviously reduces, and helps practicing thrift cost; Filled up the blank that China produces Xylitol with bamboo, the road of having opened up a new raw material for wood sugar, Xylitol production.
Wood sugar preparation method in the above-mentioned patent documentation can only be directed against with bamboo feedstock production wood sugar; And the raw material of bamboo raw material and existing aforementioned introduction has technical process long; Raw material availability is low, and the shortcoming that the utilization of resources is more is directly used bamboo feedstock production wood sugar; A large amount of consumption resource, destroy ecotope.
Viscose fiber is to be raw material with natural cellulose (pulp); Be converted into cellulose xanthate solution and spin the regenerated cellulose fibre that forms again, its production technique is following: pulp mixing → dipping → squeezing → pulverizing → experienced → yellow → dissolving → mixing → filtration → deaeration → washing → desulfurization → bleaching → pickling → oil → drying.Wherein squeezing process is to extrude unnecessary alkali in the dissolving pulp, to remove semicellulose and impurity, improves soda cellulose purity, reaches the purpose that reduces the yellow side reaction.
Prove through experimental study, in the squeezing process that viscose fiber is produced, can produce a large amount of squeezing waste alkali lye.Experiment finds that press lye after membrane filtration reclaims the part alkali in the press lye, contains a large amount of semicelluloses in the last filtering alkali lye, be rich in pentosan in its semicellulose, but the semicellulose in the squeezing salkali waste also of no use is now produced the report of wood sugar.
And the preparation method in the above-mentioned patent also is inappropriate for the squeezing waste lye that is used for from production process of viscose fiber and prepares wood sugar, and major cause is that alkali content is high in the squeezing salkali waste, and hemicellulose level is high, the low characteristics many with foreign matter content of content of lignin.
Summary of the invention
The present invention is intended to solve the bamboo of preparation wood sugar in the prior art and the shortcoming that other raw materials are nervous, resource utilization is not high; And viscose fiber prepares the social environment problem that a large amount of dischargings of the waste lye that produces in the process are brought; With the preparation of cellulose viscose fiber in the bamboo pulp; The semicellulose of dissolving in the waste lye be as the raw material of producing wood sugar, for the raw material sources of wood sugar provide an approach, and also how to utilize for the squeezing waste lye in the production process of viscose fiber; The preparation wood sugar provides a kind of novel method, reaches the effect of refuse reclamation.
In order to reach the foregoing invention purpose, its concrete technical scheme is following:
A kind of utilization squeezed the method that waste lye prepares wood sugar in the production process of viscose fiber, it is characterized in that: comprise following process step:
The preparation of A, hemicellulose solution:
The squeezing waste lye that will contain alkali and semicellulose passes through pre-filtering, secondary filter and membrane filtration successively, to see through liquid and concentrated alkali lye, makes that alkali content is 120～230g/L in the concentrated alkali lye that is obtained, and hemicellulose level is 40～70g/L;
Alkali concn is 120～230g/L in the described squeezing waste lye, and semicellulose concentration is 20～30g/L;
Flame filter press is adopted in described pre-filtering, and separating precision is 5 μ～100 μ.
Described secondary filter adopts micro-filtration to filter, and separating precision is 0.1 μ～10 μ.
Described membrane filtration adopts the nf membrane straining installation, and one or both materials in PS membrane, PET, the poly tetrafluoroethylene adopt the mode of cross flow filter to filter as the membrane filtration material, and its working pressure is 0.6～2MPa, and filtration temperature is 30～70 ℃.
The extraction of B, semicellulose:
With the concentrated alkali lye that obtains in the steps A, the pH value of at room temperature using 98.5% the vitriol oil to regulate supernatant is 4～5, this moment the liquid phase muddiness; Add 95% industrial alcohol that concentrates 2～3 times of volumes of alkali lye then; Staticly settle, filter, use the 95% industrial alcohol washing that concentrates 0.5～1 times of volume of alkali lye and be 0.08～0.1Mpa in vacuum tightness; Drying temperature is to be dried to constant weight under 60～80 ℃, obtains the semicellulose powder of white;
The hydrolysis of C, semicellulose:
The semicellulose powder that obtains among the step B is processed the semicellulose aqueous solution, add 98.5% the vitriol oil and be hydrolyzed, make hydrolysis of hemicellulose become monose;
Described hydrolysising condition is that the mass ratio of semicellulose powder and water is 1:4～1:15.
Said 98.5% sulfuric acid consumption is 1～3% of a semicellulose aqueous solution quality, 105～125 ℃ of hydrolysis temperatures, and hydrolysis time 1.5～3.5 h after hydrolysis finishes, obtain the wood sugar mass percentage concentration and are 3～8% hydrolyzed solution.
Hydrolysis reaches as far as possible semicellulose is converted into monose, improves the wood sugar productive rate;
Hydrolysis temperature is too high or hydrolysis time is long, and wood sugar can continue dehydration and generate furfural or further be hydrolyzed to low carbohydrate, like acetic acid, acetone etc., for follow-up purification process brings difficulty; Temperature crosses low or hydrolysis time is too short then causes hydrolysis incomplete;
D, in and depickling:
In the hydrolyzed solution that step C obtains, add neutralization reagent, add-on is 0.5～1.0% of a hydrolyzed solution quality, obtains throw out after the neutralization, and the elimination deposition obtains the depickling hydrolyzed solution;
Described neutralization reagent can be the multiple of a kind of or arbitrary proportion in lime carbonate, calcium hydroxide, Calcium hydrogen carbonate, the quicklime.
The purpose of neutralizing treatment is the mineral acid of removing in the hydrolyzed solution, sloughs the xylose crystalline adverse factors.
E, pre-concentration:
Depickling hydrolyzed solution among the step D is carried out the vacuum decompression evaporation concentration;
Described vacuum tightness is 0.08～0.1MPa, and temperature is 75～80 ℃, and the evaporation concentration time is 30～60min; The wood sugar concentration expressed in percentage by weight of depickling hydrolyzed solution is brought up to 30～35%, obtain syrup;
Among the step D with depickling after the contained sugared concentration of depickling hydrolyzed solution lower (3～8%) that obtains; Need through the vacuum decompression evaporation concentration; Make the sugared concentration behind the hydrolyzed solution bring up to 30～35%, this step can also further be removed sulfate ion, and the calcium sulphate crystal of separating out is removed.
F, decolouring:
With the syrup that obtains through pre-concentration in the step e processing of decolouring;
In temperature is under 75～80 ℃, adds the gac of syrup weight 7～10%, and 30～40min is handled in decolouring, and making its pH value is 2～3, obtains transparency at last and be 30～40% syrup.
Syrup color and luster behind the pre-concentration is darker, the processing of need decolouring, and normal pressure adopts the decolorizing with activated carbon method, removes pigment colloid and the nitrogenous thing of part in the hydrolyzed solution.
G, IX:
The syrup that obtains through decolouring in the step F is carried out conventional ion exchange treatment, obtain purity 95～97%, specific conductivity is smaller or equal to the xylose solution of 10 μ s/cm.
Ion exchange treatment is specially:
Resin cation(R.C.) and the supporting use of resin anion(R.A) are selected in IX for use, and ion-exchange temperature is 30～40 ℃, earlier through positive post, after cloudy post again through positive post, gets scavenging solution.After quantitative material is thrown and finished, replace till the sugar-free with pure water, water recoils from bottom to top then again, makes that resin layer is loose to be stirred, and removes upper strata impurity through press over system, then with acid, alkali regeneration, regenerates with pure water at last.
It is 0.5h that the sun resin regeneration is used ionized water back flushing, time earlier, the H with 2.3%
2SO
4(or 2% hydrochloric acid) solution is regenerated from bottom to top, when effluent differs 0.2% with the acid concentration that adds liquid, stops to add acid, closes bottom acid inlet valve door, soaks 1h again, goes into pond for recovering through soak solution.
It is 0.5h that negative resin regeneration is used ionized water back flushing, time earlier, and the pH value is about 6, with the Na that adopts 4.5%
2CO
3Regeneration (or sodium hydroxide of 2%) solution is regenerated from bottom to top, when the concentration of lye of effluent and adding differs 0.2%, stops to add alkali, closes bottom alkali-feeding valve door, soaks 1h again, and soak solution is gone into pond for recovering.
The purpose of this road technology is further to purify syrup, and the purity of handling wood sugar in the xylose solution of back can reach 95～97%, makes xylose solution be the water white transparency shape, whole cleansing cycles 26～28h.
H, with the xylose solution among the step G carry out that routine concentrates, crystallization, separation, drying process obtain the wood sugar finished product.
Xylose solution after the IX adopts vacuum concentration, and two steps of evaporation concentration carry out:
The first step is 0.06～0.08Mpa in vacuum tightness, and temperature is under 50～55 ℃ the situation, and being concentrated to the weight percent that wood sugar accounts for xylose solution is 25～30%;
Second step was used lift-film evaporator, and vacuum tightness is brought up to 0.08～0.1Mpa, 65～70 ℃ of temperature, and being concentrated to the weight percent that wood sugar accounts for xylose solution is 75～80%, promptly can discharging, be pressed into crystallizer;
Xylose solution temperature after concentrating drops to 60～65 ℃ and adds crystal seed, slowly stirs crystallization in motion, per hour lowers the temperature 1 ℃; When exceeding 1～10 ℃ than room temperature, the promptly separable xylose crystalline body of obtaining adopts 75～80 ℃ then; Vacuum tightness 0.08Mpa, time of drying 2～4, h carried out drying, obtained the wood sugar finished product; Gained finished product crystalline xylose moisture≤5.0%, wood sugar purity>=95% in the total solid.
The useful technique effect that the present invention brings:
1, at the preparatory phase of hemicellulose solution, owing to adopted membrane technique to concentrate hemicellulose solution, having saved with traditional raw material is basic needed preprocessing process-promptly wash, high temperature steaming process.The contrast traditional raw material is the wood sugar preparation technology on basis, and membrane technique has remarkable advantages at aspects such as energy-saving and environmental protection, material consumption, occupations of land, has also avoided traditional raw material in preprocessing process, to produce a large amount of waste residues simultaneously, has caused the incident of contaminate environment to take place.
2, in extraction stage of semicellulose; The technology that need not adopt centrifugal separation process to remove the technology of residue in the traditional raw material and directly adopt vitriol oil regulator solution pH value, ethanol to separate out, wash semicellulose; This has practiced thrift the problem of the inclined to one side alkali of subsequent wastewater treatment on the one hand, can utilize its tart waste water to neutralize simultaneously and regulate the problem of alkaline waste water.In addition, this step adopts ethanol to separate out, wash the purity height of semicellulose required time weak point, gained semicellulose, have the high characteristics of efficient; Only needing simple distil process is recyclable ethanol, reaches the purpose of resources of production cyclically utilizing.
3, at the hydrolysis stage of semicellulose; Because having adopted viscose glue squeezing waste lye is raw material; The semicellulose that is extracted is Powdered; It is that the bath raio of fundamental technology is slightly larger that hydrolysis bath under the acidic conditions is compared traditional raw material, and under equal conditions, the hydrolysis degree of the semicellulose that this method is prepared is that the hydrolysis degree of the prepared semicellulose in basis is more thorough with the traditional raw material.Therefore, at this hydrolysis stage, be the consumption that reduced the energy of the hydrolysis of hemicellulose technology of raw material, reduced operation steps, improved working efficiency with the viscose glue press lye.
4, in depickling, pre-concentration, decolouring, IX and concentrate, crystallization, separate drying and other steps with conventional preparation process is similar, have good production compatibility.Therefore, do not need bigger technological transformation and device customizing, also need not retrain the employee, have stronger actual motion and be worth.
5, adopt technical scheme of the present invention; Can utterly destroy the objectionable impurities of contaminate environment such as the salkali waste that produces in the viscose glue production process, waste water; Can reach the standard of whole process cleaner production; Make viscose glue manufacturing enterprise when producing viscose glue, also can produce wood sugar simultaneously, also accomplished refuse reclamation when reaching the environmental protection purpose.
Embodiment
Embodiment 1
A kind of utilization squeezed the method that waste lye prepares wood sugar in the production process of viscose fiber, comprise following process step:
The preparation of A, hemicellulose solution: the squeezing waste lye that will contain alkali and semicellulose passes through pre-filtering, secondary filter and membrane filtration successively, obtains to see through liquid and concentrated alkali lye, and alkali content is 120g/L in the concentrated alkali lye, and hemicellulose level is 40g/L;
The extraction of B, semicellulose: with the concentrated alkali lye that obtains in the steps A; The pH value of the vitriol oil of use 98.5% adjusting supernatant is 4 under the room temperature, and this adds 95% industrial alcohol that concentrates 2 times of volumes of alkali lye then, staticly settles; Filter; Use the 95% industrial alcohol washing of concentrated 0.5 times of volume of alkali lye and be 0.08Mpa in vacuum tightness, drying temperature is to be dried to constant weight under 60 ℃, obtains the semicellulose powder of white;
The hydrolysis of C, semicellulose: the semicellulose powder that obtains among the step B is processed the semicellulose aqueous solution, add 98.5% the vitriol oil and be hydrolyzed; The mass ratio of said semicellulose powder and water is 1:4; Said 98.5% sulfuric acid consumption is 1% of a semicellulose aqueous solution quality, 105 ℃ of hydrolysis temperatures, and hydrolysis time 1.5 h obtain the wood sugar mass percentage concentration and are 3% hydrolyzed solution;
D, in and depickling: in the hydrolyzed solution that step C obtains, add neutralization reagent carry out in and depickling, obtain deposition after the neutralization, the elimination deposition obtains the depickling hydrolyzed solution;
E, pre-concentration: the depickling hydrolyzed solution among the step D is carried out the vacuum decompression evaporation concentration, obtain the wood sugar concentration expressed in percentage by weight and be 30% syrup;
F, decolouring:, obtain transparency and be 30% syrup with the syrup that obtains through pre-concentration in the step e processing of decolouring;
G, IX: the syrup that obtains through decolouring in the step F is carried out conventional ion exchange treatment, and the purity that obtains wood sugar is 95%, and specific conductivity is smaller or equal to the xylose solution of 10 μ s/cm;
H, with the xylose solution among the step G carry out that routine concentrates, crystallization, separation, drying process obtain the wood sugar finished product.
Alkali concn is 120g/L in the squeezing waste lye described in the steps A, and semicellulose concentration is 20g/L.
Adopt flame filter press in the pre-filtering described in the steps A, separating precision is 5 μ.
Adopt micro-filtration to filter in the secondary filter described in the steps A, separating precision is 0.1 μ.
Adopt the nf membrane straining installation at the membrane filtration described in the steps A; One or both materials in PS membrane, PET, the poly tetrafluoroethylene are as the membrane filtration material; Adopt the mode of cross flow filter to filter, its working pressure is 0.6MPa, and filtration temperature is 30 ℃.
Add-on at the neutralization reagent described in the step D is 0.5% of a hydrolyzed solution quality.
Above-mentioned neutralization reagent is a kind of or arbitrary proportion multiple in lime carbonate, calcium hydroxide, Calcium hydrogen carbonate, the quicklime.
Be specially at vacuum tightness 0.08MPa at pre-concentration described in the step e, under 75 ℃ of the temperature, evaporation concentration 30min.
Be specially under 75 ℃ of temperature in the decolouring described in the step F, add the gac of syrup weight 7%, 30min is handled in decolouring, and making its pH value is 2.
Embodiment 2
A kind of utilization squeezed the method that waste lye prepares wood sugar in the production process of viscose fiber, comprise following process step:
The preparation of A, hemicellulose solution: the squeezing waste lye that will contain alkali and semicellulose passes through pre-filtering, secondary filter and membrane filtration successively, obtains to see through liquid and concentrated alkali lye, and alkali content is 230g/L in the concentrated alkali lye, and hemicellulose level is 70g/L;
The extraction of B, semicellulose: with the concentrated alkali lye that obtains in the steps A; The pH value of the vitriol oil of use 98.5% adjusting supernatant is 5 under the room temperature, and this adds 95% industrial alcohol that concentrates 3 times of volumes of alkali lye then, staticly settles; Filter; Use the 95% industrial alcohol washing of concentrated 1 times of volume of alkali lye and be 0.1Mpa in vacuum tightness, drying temperature is to be dried to constant weight under 80 ℃, obtains the semicellulose powder of white;
The hydrolysis of C, semicellulose: the semicellulose powder that obtains among the step B is processed the semicellulose aqueous solution, add 98.5% the vitriol oil and be hydrolyzed; The mass ratio of said semicellulose powder and water is 1:15; Said 98.5% sulfuric acid consumption is 3% of a semicellulose aqueous solution quality, 125 ℃ of hydrolysis temperatures, and hydrolysis time 3.5 h obtain the wood sugar mass percentage concentration and are 8% hydrolyzed solution;
D, in and depickling: in the hydrolyzed solution that step C obtains, add neutralization reagent carry out in and depickling, obtain deposition after the neutralization, the elimination deposition obtains the depickling hydrolyzed solution;
E, pre-concentration: the depickling hydrolyzed solution among the step D is carried out the vacuum decompression evaporation concentration, obtain the wood sugar concentration expressed in percentage by weight and be 35% syrup;
F, decolouring:, obtain transparency and be 40% syrup with the syrup that obtains through pre-concentration in the step e processing of decolouring;
G, IX: the syrup that obtains through decolouring in the step F is carried out conventional ion exchange treatment, and the purity that obtains wood sugar is 97%, and specific conductivity is smaller or equal to the xylose solution of 10 μ s/cm;
H, with the xylose solution among the step G carry out that routine concentrates, crystallization, separation, drying process obtain the wood sugar finished product.
Alkali concn is 230g/L in the squeezing waste lye described in the steps A, and semicellulose concentration is 30g/L.
Adopt flame filter press in the pre-filtering described in the steps A, separating precision is 100 μ.
Adopt micro-filtration to filter in the secondary filter described in the steps A, separating precision is 10 μ.
Adopt the nf membrane straining installation at the membrane filtration described in the steps A, one or both materials in PS membrane, PET, the poly tetrafluoroethylene adopt the mode of cross flow filter to filter as the membrane filtration material, and its working pressure is 2MPa, and filtration temperature is 70 ℃.
Add-on at the neutralization reagent described in the step D is 1.0% of a hydrolyzed solution quality.
Above-mentioned neutralization reagent is a kind of or arbitrary proportion multiple in lime carbonate, calcium hydroxide, Calcium hydrogen carbonate, the quicklime.
Be specially at vacuum tightness 0.1MPa at pre-concentration described in the step e, under 80 ℃ of the temperature, evaporation concentration 60min.
Be specially under 80 ℃ of temperature in the decolouring described in the step F, add the gac of syrup weight 10%, 40min is handled in decolouring, and making its pH value is 3.
Embodiment 3
A kind of utilization squeezed the method that waste lye prepares wood sugar in the production process of viscose fiber, comprise following process step:
The preparation of A, hemicellulose solution: the squeezing waste lye that will contain alkali and semicellulose passes through pre-filtering, secondary filter and membrane filtration successively, obtains to see through liquid and concentrated alkali lye, and alkali content is 175g/L in the concentrated alkali lye, and hemicellulose level is 55g/L;
The extraction of B, semicellulose: with the concentrated alkali lye that obtains in the steps A; The pH value of the vitriol oil of use 98.5% adjusting supernatant is 4.5 under the room temperature, and this adds 95% industrial alcohol that concentrates 2.5 times of volumes of alkali lye then, staticly settles; Filter; Use the 95% industrial alcohol washing of concentrated 0.75 times of volume of alkali lye and be 0.09Mpa in vacuum tightness, drying temperature is to be dried to constant weight under 70 ℃, obtains the semicellulose powder of white;
The hydrolysis of C, semicellulose: the semicellulose powder that obtains among the step B is processed the semicellulose aqueous solution, add 98.5% the vitriol oil and be hydrolyzed; The mass ratio of said semicellulose powder and water is 1:9.5; Said 98.5% sulfuric acid consumption is 2% of a semicellulose aqueous solution quality, 115 ℃ of hydrolysis temperatures, and hydrolysis time 2.5 h obtain the wood sugar mass percentage concentration and are 5.5% hydrolyzed solution;
D, in and depickling: in the hydrolyzed solution that step C obtains, add neutralization reagent carry out in and depickling, obtain deposition after the neutralization, the elimination deposition obtains the depickling hydrolyzed solution;
E, pre-concentration: the depickling hydrolyzed solution among the step D is carried out the vacuum decompression evaporation concentration, obtain the wood sugar concentration expressed in percentage by weight and be 32.5% syrup;
F, decolouring:, obtain transparency and be 35% syrup with the syrup that obtains through pre-concentration in the step e processing of decolouring;
G, IX: the syrup that obtains through decolouring in the step F is carried out conventional ion exchange treatment, and the purity that obtains wood sugar is 96%, and specific conductivity is smaller or equal to the xylose solution of 10 μ s/cm;
H, with the xylose solution among the step G carry out that routine concentrates, crystallization, separation, drying process obtain the wood sugar finished product.
Alkali concn is 175g/L in the squeezing waste lye described in the steps A, and semicellulose concentration is 25g/L.
Adopt flame filter press in the pre-filtering described in the steps A, separating precision is 52.5 μ.
Adopt micro-filtration to filter in the secondary filter described in the steps A, separating precision is 5.05 μ.
Adopt the nf membrane straining installation at the membrane filtration described in the steps A; One or both materials in PS membrane, PET, the poly tetrafluoroethylene are as the membrane filtration material; Adopt the mode of cross flow filter to filter, its working pressure is 1.3MPa, and filtration temperature is 50 ℃.
Add-on at the neutralization reagent described in the step D is 0.75% of a hydrolyzed solution quality.
Above-mentioned neutralization reagent is a kind of or arbitrary proportion multiple in lime carbonate, calcium hydroxide, Calcium hydrogen carbonate, the quicklime.
Be specially at vacuum tightness 0.09MPa at pre-concentration described in the step e, under 77.5 ℃ of the temperature, evaporation concentration 45min.
Be specially under 77.5 ℃ of temperature in the decolouring described in the step F, add the gac of syrup weight 8.5%, 35min is handled in decolouring, and making its pH value is 2.5.
Embodiment 4
A kind of utilization squeezed the method that waste lye prepares wood sugar in the production process of viscose fiber, comprise following process step:
The preparation of A, hemicellulose solution: the squeezing waste lye that will contain alkali and semicellulose passes through pre-filtering, secondary filter and membrane filtration successively, obtains to see through liquid and concentrated alkali lye, and alkali content is 215g/L in the concentrated alkali lye, and hemicellulose level is 46g/L;
The extraction of B, semicellulose: with the concentrated alkali lye that obtains in the steps A; The pH value of the vitriol oil of use 98.5% adjusting supernatant is 5 under the room temperature, and this adds 95% industrial alcohol that concentrates 2.2 times of volumes of alkali lye then, staticly settles; Filter; Use the 95% industrial alcohol washing of concentrated 0.93 times of volume of alkali lye and be 0.095Mpa in vacuum tightness, drying temperature is to be dried to constant weight under 71 ℃, obtains the semicellulose powder of white;
The hydrolysis of C, semicellulose: the semicellulose powder that obtains among the step B is processed the semicellulose aqueous solution, add 98.5% the vitriol oil and be hydrolyzed; The mass ratio of said semicellulose powder and water is 1:5.5; Said 98.5% sulfuric acid consumption is 1.3% of a semicellulose aqueous solution quality, 119 ℃ of hydrolysis temperatures, and hydrolysis time 3.2 h obtain the wood sugar mass percentage concentration and are 7.9% hydrolyzed solution;
D, in and depickling: in the hydrolyzed solution that step C obtains, add neutralization reagent carry out in and depickling, obtain deposition after the neutralization, the elimination deposition obtains the depickling hydrolyzed solution;
E, pre-concentration: the depickling hydrolyzed solution among the step D is carried out the vacuum decompression evaporation concentration, obtain the wood sugar concentration expressed in percentage by weight and be 31.5% syrup;
F, decolouring:, obtain transparency and be 33% syrup with the syrup that obtains through pre-concentration in the step e processing of decolouring;
G, IX: the syrup that obtains through decolouring in the step F is carried out conventional ion exchange treatment, and the purity that obtains wood sugar is 96.8%, and specific conductivity is smaller or equal to the xylose solution of 10 μ s/cm;
H, with the xylose solution among the step G carry out that routine concentrates, crystallization, separation, drying process obtain the wood sugar finished product.
Alkali concn is 215g/L in the squeezing waste lye described in the steps A, and semicellulose concentration is 26g/L.
Adopt flame filter press in the pre-filtering described in the steps A, separating precision is 40 μ.
Adopt micro-filtration to filter in the secondary filter described in the steps A, separating precision is 8 μ.
Adopt the nf membrane straining installation at the membrane filtration described in the steps A; One or both materials in PS membrane, PET, the poly tetrafluoroethylene are as the membrane filtration material; Adopt the mode of cross flow filter to filter, its working pressure is 1.7MPa, and filtration temperature is 34 ℃.
Add-on at the neutralization reagent described in the step D is 0.77% of a hydrolyzed solution quality.
Above-mentioned neutralization reagent is a kind of or arbitrary proportion multiple in lime carbonate, calcium hydroxide, Calcium hydrogen carbonate, the quicklime.
Be specially at vacuum tightness 0.09MPa at pre-concentration described in the step e, under 77 ℃ of the temperature, evaporation concentration 58min.
Be specially under 79 ℃ of temperature in the decolouring described in the step F, add the gac of syrup weight 8.5%, 33min is handled in decolouring, and making its pH value is 2.8.
Embodiment 5
Ion exchange treatment is specially:
Resin cation(R.C.) and the supporting use of resin anion(R.A) are selected in IX for use, and ion-exchange temperature is 30～40 ℃, earlier through positive post, after cloudy post again through positive post, gets scavenging solution.After quantitative material is thrown and finished, replace till the sugar-free with pure water, water recoils from bottom to top then again, makes that resin layer is loose to be stirred, and removes upper strata impurity through press over system, then with acid, alkali regeneration, regenerates with pure water at last.
It is 0.5h that the sun resin regeneration is used ionized water back flushing, time earlier, the H with 2.3%
2SO
4(or 2% hydrochloric acid) solution is regenerated from bottom to top, when effluent differs 0.2% with the acid concentration that adds liquid, stops to add acid, closes bottom acid inlet valve door, soaks 1h again, goes into pond for recovering through soak solution.
It is 0.5h that negative resin regeneration is used ionized water back flushing, time earlier, and the pH value is about 6, with the Na that adopts 4.5%
2CO
3Regeneration (or sodium hydroxide of 2%) solution is regenerated from bottom to top, when the concentration of lye of effluent and adding differs 0.2%, stops to add alkali, closes bottom alkali-feeding valve door, soaks 1h again, and soak solution is gone into pond for recovering.
The purpose of this road technology is further to purify syrup, and the purity of handling wood sugar in the xylose solution of back can reach 95～97%, makes xylose solution be the water white transparency shape, whole cleansing cycles 26～28h.
Embodiment 6
Xylose solution carries out that routine concentrates, crystallization, separation, drying process obtain the wood sugar finished product.
Xylose solution after the IX adopts vacuum concentration, and two steps of evaporation concentration carry out:
The first step is 0.06Mpa in vacuum tightness, and temperature is under 50 ℃ the situation, and being concentrated to the weight percent that wood sugar accounts for xylose solution is 25%;
Second step was used lift-film evaporator, and vacuum tightness is brought up to 0.08Mpa, 65 ℃ of temperature, and being concentrated to the weight percent that wood sugar accounts for xylose solution is 75%, promptly can discharging, be pressed into crystallizer;
Xylose solution temperature after concentrating drops to 60 ℃ and adds crystal seed, slowly stirs crystallization in motion, per hour lowers the temperature 1 ℃; When exceeding 1 ℃ than room temperature, the promptly separable xylose crystalline body of obtaining adopts 75 ℃ then; Vacuum tightness 0.08Mpa, time of drying, 2h carried out drying, obtained the wood sugar finished product; Gained finished product crystalline xylose moisture≤5.0%, wood sugar purity>=95% in the total solid.
Embodiment 7
Xylose solution carries out that routine concentrates, crystallization, separation, drying process obtain the wood sugar finished product.
Xylose solution after the IX adopts vacuum concentration, and two steps of evaporation concentration carry out:
The first step is 0.08Mpa in vacuum tightness, and temperature is under 55 ℃ the situation, and being concentrated to the weight percent that wood sugar accounts for xylose solution is 30%;
Second step was used lift-film evaporator, and vacuum tightness is brought up to 0.1Mpa, 70 ℃ of temperature, and being concentrated to the weight percent that wood sugar accounts for xylose solution is 80%, promptly can discharging, be pressed into crystallizer;
Xylose solution temperature after concentrating drops to 65 ℃ and adds crystal seed, slowly stirs crystallization in motion, per hour lowers the temperature 1 ℃; When exceeding 10 ℃ than room temperature, the promptly separable xylose crystalline body of obtaining adopts 80 ℃ then; Vacuum tightness 0.08Mpa, time of drying 4, h carried out drying, obtained the wood sugar finished product; Gained finished product crystalline xylose moisture≤5.0%, wood sugar purity>=95% in the total solid.
Embodiment 8
Xylose solution carries out that routine concentrates, crystallization, separation, drying process obtain the wood sugar finished product.
Xylose solution after the IX adopts vacuum concentration, and two steps of evaporation concentration carry out:
The first step is 0.07Mpa in vacuum tightness, and temperature is under 52.5 ℃ the situation, and being concentrated to the weight percent that wood sugar accounts for xylose solution is 27.5%;
Second step was used lift-film evaporator, and vacuum tightness is brought up to 0.09Mpa, 67.5 ℃ of temperature, and being concentrated to the weight percent that wood sugar accounts for xylose solution is 77.5%, promptly can discharging, be pressed into crystallizer;
Xylose solution temperature after concentrating drops to 62.5 ℃ and adds crystal seed, slowly stirs crystallization in motion, per hour lowers the temperature 1 ℃; When exceeding 5.5 ℃ than room temperature, the promptly separable xylose crystalline body of obtaining adopts 77.5 ℃ then; Vacuum tightness 0.08Mpa, time of drying 3, h carried out drying, obtained the wood sugar finished product; Gained finished product crystalline xylose moisture≤5.0%, wood sugar purity>=95% in the total solid.
Embodiment 9
Xylose solution carries out that routine concentrates, crystallization, separation, drying process obtain the wood sugar finished product.
Xylose solution after the IX adopts vacuum concentration, and two steps of evaporation concentration carry out:
The first step is 0.077Mpa in vacuum tightness, and temperature is under 51 ℃ the situation, and being concentrated to the weight percent that wood sugar accounts for xylose solution is 29%;
Second step was used lift-film evaporator, and vacuum tightness is brought up to 0.095Mpa, 68 ℃ of temperature, and being concentrated to the weight percent that wood sugar accounts for xylose solution is 77%, promptly can discharging, be pressed into crystallizer;
Xylose solution temperature after concentrating drops to 63.5 ℃ and adds crystal seed, slowly stirs crystallization in motion, per hour lowers the temperature 1 ℃; When exceeding 2 ℃ than room temperature, the promptly separable xylose crystalline body of obtaining adopts 79 ℃ then; Vacuum tightness 0.08Mpa, time of drying 3.5, h carried out drying, obtained the wood sugar finished product; Gained finished product crystalline xylose moisture≤5.0%, wood sugar purity>=95% in the total solid.
Claims (9)
1. method of utilizing in the production process of viscose fiber squeezing waste lye to prepare wood sugar is characterized in that: comprise following process step:
The preparation of A, hemicellulose solution: the squeezing waste lye that will contain alkali and semicellulose passes through pre-filtering, secondary filter and membrane filtration successively; Obtain to see through liquid and concentrated alkali lye; Alkali content is 120～230g/L in the concentrated alkali lye, and hemicellulose level is 40～70g/L;
The extraction of B, semicellulose: with the concentrated alkali lye that obtains in the steps A; The pH value of the vitriol oil of use 98.5% adjusting supernatant is 4～5 under the room temperature, and this adds 95% industrial alcohol that concentrates 2～3 times of volumes of alkali lye then, staticly settles; Filter; Use to concentrate the 95% industrial alcohol washing of 0.5～1 times of volume of alkali lye and be 0.08～0.1Mpa in vacuum tightness, drying temperature is to be dried to constant weight under 60～80 ℃, obtains the semicellulose powder of white;
The hydrolysis of C, semicellulose: the semicellulose powder that obtains among the step B is processed the semicellulose aqueous solution, add 98.5% the vitriol oil and be hydrolyzed; The mass ratio of said semicellulose powder and water is 1:4～1:15; Said 98.5% sulfuric acid consumption is 1～3% of a semicellulose aqueous solution quality, 105～125 ℃ of hydrolysis temperatures, and hydrolysis time 1.5～3.5 h obtain the wood sugar mass percentage concentration and are 3～8% hydrolyzed solution;
D, in and depickling: in the hydrolyzed solution that step C obtains, add neutralization reagent carry out in and depickling, obtain deposition after the neutralization, the elimination deposition obtains the depickling hydrolyzed solution;
E, pre-concentration: the depickling hydrolyzed solution among the step D is carried out the vacuum decompression evaporation concentration, obtain the wood sugar concentration expressed in percentage by weight and be 30～35% syrup;
F, decolouring:, obtain transparency and be 30～40% syrup with the syrup that obtains through pre-concentration in the step e processing of decolouring;
G, IX: the syrup that obtains through decolouring in the step F is carried out conventional ion exchange treatment, and the purity that obtains wood sugar is 95～97%, and specific conductivity is smaller or equal to the xylose solution of 10 μ s/cm;
H, with the xylose solution among the step G carry out that routine concentrates, crystallization, separation, drying process obtain the wood sugar finished product.
2. a kind of utilization the according to claim 1 squeezed the method that waste lye prepares wood sugar in the production process of viscose fiber, it is characterized in that: alkali concn is 120～230g/L in the squeezing waste lye described in the steps A, and semicellulose concentration is 20～30g/L.
3. a kind of utilization the according to claim 1 squeezed the method that waste lye prepares wood sugar in the production process of viscose fiber, it is characterized in that: adopt flame filter press in the pre-filtering described in the steps A, separating precision is 5 μ～100 μ.
4. a kind of utilization the according to claim 1 squeezed the method that waste lye prepares wood sugar in the production process of viscose fiber, it is characterized in that: adopt micro-filtration to filter in the secondary filter described in the steps A, separating precision is 0.1 μ～10 μ.
5. a kind of utilization the according to claim 1 squeezed the method that waste lye prepares wood sugar in the production process of viscose fiber; It is characterized in that: adopt the nf membrane straining installation at the membrane filtration described in the steps A; One or both materials in PS membrane, PET, the poly tetrafluoroethylene are as the membrane filtration material; Adopt the mode of cross flow filter to filter, its working pressure is 0.6～2MPa, and filtration temperature is 30～70 ℃.
6. a kind of utilization the according to claim 1 squeezed the method that waste lye prepares wood sugar in the production process of viscose fiber, it is characterized in that: the add-on at the neutralization reagent described in the step D is 0.5～1.0% of a hydrolyzed solution quality.
7. a kind of method of utilizing in the production process of viscose fiber squeezing waste lye to prepare wood sugar according to claim 6 is characterized in that: described neutralization reagent is a kind of or arbitrary proportion multiple in lime carbonate, calcium hydroxide, Calcium hydrogen carbonate, the quicklime.
8. a kind of utilization the according to claim 1 squeezed the method that waste lye prepares wood sugar in the production process of viscose fiber; It is characterized in that: be specially at vacuum tightness 0.08～0.1MPa at pre-concentration described in the step e; Under 75～80 ℃ of the temperature, evaporation concentration 30～60min.
9. a kind of utilization the according to claim 1 squeezed the method that waste lye prepares wood sugar in the production process of viscose fiber; It is characterized in that: be specially under 75～80 ℃ of temperature in the decolouring described in the step F; The gac that adds syrup weight 7～10%; 30～40min is handled in decolouring, and making its pH value is 2～3.
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