CN103074454B - Method for preparing D-xylose and L-arabinose by recycling phosphoric acid - Google Patents
Method for preparing D-xylose and L-arabinose by recycling phosphoric acid Download PDFInfo
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Abstract
The invention discloses a method for preparing D-xylose and L-arabinose by recycling phosphoric acid. With bagasse, bagasse pith or sugarcane tops as raw materials, the D-xylose and the L-arabinose are prepared by hydrolyzing the raw materials, precipitating phosphate radicals of hydrolysate and purifying; and with combination of a cane sugar manufacture process, after being subjected to acid dissolution treatment, phosphate radical precipitates are added into cane juice as a processing aid, which is obliged to be used in the cane sugar manufacture process, for recycling. The method disclosed by the invention is good for environment protection and recycling in the cane sugar manufacture industry, and compared with an xylose production method adopting sulfuric acid or hydrochloric acid at present, the method has the advantages of no hydrolytic acid pollution, simplicity and convenience in process operation, high yield of the D-xylose and L-arabinose, and low cost, and is suitable for industrial production and good for solving the problem of bottleneck restriction of environment pollution in xylose production.
Description
Technical field
The invention belongs to technical field of functional sugar, relate in particular to the protection of cane sugar manufacture industrial environment and resource circulation utilization.Specifically a kind of recycling phosphoric acid prepares the method for D-wood sugar, L-arabinose.
Background technology
The D-wood sugar belongs to five-carbon ring aldehydo sugar, has good biological function, if by human body, do not digested, noenergy, can be used as non-caloric sweetener, is applicable to obese person and diabetic subject, in the activating human body enteron aisle, bifidus bacillus short its growth, improve the human body microenvironment, improves body immunity; By oral microorganism, do not utilized, have the part physiological function of food fibre, can reduce serum cholesterol, have good nourishing function.L-arabinose is also a kind of rare functional sugar, has and suppresses fat, the effects such as auxiliary hyperglycemic, reducing blood-fat.
Chinese patent 200910039185.6 discloses a kind of method for preparing the plant hemicellulose hydrolyzed solution and extract wood sugar and pectinose, in production process, used a large amount of organic solvents, production cost is high, easily to environment, and complicated operation, be difficult to realize industrialization.
Domestic preparation D-wood sugar, L-arabinose now mainly concentrate on the north, mainly with waste crop materials such as corn cob, maize peels, it is raw material, the hydrolysis that the industrialization acid system prepares D-wood sugar, L-arabinose is sulfuric acid with acid, at present because environmental protection pressure has the trend of using hydrochloric acid instead, adopt the ion exchange method desalination, need to just can reach requirement through anion and cation exchange resin repeatedly, the resin demand is large, and clean and need large-scale purification water, regeneration needs to consume a large amount of soda acids, the generation waste liquid is many, complex operation.
Therefore a kind of technical process of needs is easy, production cost is low, the resource reusable edible, and acid-base waste fluid is few, is suitable for the method for suitability for industrialized production D-wood sugar, L-arabinose.
Summary of the invention
The object of the present invention is to provide a kind of production cost low, the resource reusable edible, do not form the hydrolysis acid pollution, and technical matters is easy, and raw material sources are D-wood sugar, L-arabinose production method widely.
The technical scheme that the present invention solves the problems of the technologies described above is as follows:
A kind of method that recycling phosphoric acid prepares D-wood sugar, L-arabinose is hydrolyzed by 1. raw materials; 2. the hydrolyzed solution phosphate radical precipitates; 3. purifying; 4. purifying elutriant phosphate radical precipitates; 5.D-the preparation of wood sugar, L-arabinose; 6. phosphoric acid resource utilization recycling operates, and concrete steps are as follows:
1. raw material hydrolysis:
It is that 3.0 ~ 8.0% phosphoric acid is hydrolyzed that bagasse, sugarcane marrow or Caulis Sacchari sinensis leaf add mass percentage concentration, and the solid-to-liquid ratio kg/L of bagasse, sugarcane marrow or Caulis Sacchari sinensis leaf weight and phosphoric acid volume is 1: 1 ~ 1: 10, and hydrolysis temperature is 110 ~ 130 ℃, and hydrolysis time is 1 ~ 5h; After being hydrolyzed, obtain hydrolysed mix, hydrolysed mix is filtered, obtain hydrolyzed solution.
2. the hydrolyzed solution phosphate radical precipitates:
In hydrolyzed solution, add milk of lime to carry out neutralization precipitation, regulate pH to 4.5 ~ 7.2, after pH is stable, the hydrolyzed solution after being neutralized and phosphate radical precipitation.Carry out solid-liquid separation, the phosphate radical precipitation is reclaimed, hydrolyzed solution is further purified.
3. purifying:
Adopt anionite-exchange resin and Zeo-karb, hydrolyzed solution is carried out to purifying, obtain the hydrolyzed solution after purifying.
4. purifying elutriant phosphate radical precipitates:
The ion exchange resin used to purifying carries out wash-out regeneration, obtains elutriant.In elutriant, adding milk of lime adjusting pH is 7.2 ~ 9.0, after pH is stable, carries out solid-liquid separation, obtains supernatant liquor and phosphate radical precipitation.The phosphate radical precipitation is reclaimed.
5.D-the preparation of wood sugar, L-arabinose:
Hydrolyzed solution after purifying, through analog stream movable bed chromatographic separation, concentrated, crystallization, prepares D-wood sugar and L-arabinose crystal.
6. the phosphoric acid resource utilization recycles:
Add phosphoric acid, sulfurous acid or stove drying to pH3.0 ~ 4.5 precipitation of the phosphate radical in step 2 and step 4, until solid all dissolves, be precipitated lysate;
Detect the phosphoric acid value of resolution of precipitate liquid, after the allotment, join in sugarcane juice and carry out the resource utilization recycling according to actual needs.
In above-mentioned steps 6, the phosphate radical precipitation adds phosphoric acid, sulfurous acid or stove drying all to dissolve, be precipitated lysate, after recovery, be applied in the cane juice clarification technique of cane sugar manufacture, phosphate radical is deposited in filter mud again, the filter mud as fertilizer sources utilizes again, realizes resource circulation utilization.
In above-mentioned steps 2, the hydrolyzed solution phosphate radical is precipitated as in hydrolyzed solution and adds milk of lime to carry out neutralization precipitation, regulates pH to 4.8 ~ 5.0, the hydrolyzed solution after being neutralized and phosphate radical precipitation.
Above-mentioned steps 4 elutriant phosphate radicals are precipitated as purifying ion exchange resin used are carried out to wash-out regeneration, obtain elutriant; In elutriant, adding milk of lime adjusting pH is 8.1, obtains supernatant liquor and phosphate radical precipitation.
Above-mentioned steps 6 phosphoric acid resource utilization recycling methods are that phosphate radical precipitation adds phosphoric acid, sulfurous acid or stove drying, regulate pH to 3.0 solid is all dissolved, and join in the sugarcane juice of cane sugar manufacture and carry out recycling.
The obtained technical progress of the present invention is:
1. the present invention is hydrolyzed phosphate radical used after precipitation, neutralization, and recycle is in the cane juice clarification technique of cane sugar manufacture, and phosphate radical again is deposited to the filter mud as fertilizer sources and again recycles, and realizes resource circulation utilization.The generation waste liquid is few, and environmental pollution is little, has saved acid and alkali consumption, reduces production costs.
2. raw material bagasse of the present invention, sugarcane marrow and Caulis Sacchari sinensis leaf wide material sources, production cost is low, the processing condition maturation, easy and simple to handle, stabilization of equipment performance is high, does not use any organic solvent, and product purity is high, is suitable for suitability for industrialized production.
Embodiment
Below by embodiment, the present invention is described in further detail.Following examples are used for the present invention is described, but are not used for limiting the scope of the invention.
Embodiment 1
The method operation steps that recycling phosphoric acid prepares D-wood sugar, L-arabinose is as follows:
1. raw material hydrolysis:
It is that 3.0% phosphoric acid is hydrolyzed that bagasse adds mass percentage concentration, and the solid-to-liquid ratio kg/L of bagasse and phosphoric acid is 1:10, and hydrolysis temperature is 110 ℃, and hydrolysis time is 5h.
After being hydrolyzed, obtain hydrolysed mix, hydrolysed mix is filtered, obtain hydrolyzed solution.
2. the hydrolyzed solution phosphate radical precipitates:
In hydrolyzed solution, add milk of lime to carry out neutralization precipitation, regulate pH to 4.5, the hydrolyzed solution after being neutralized and precipitation (being the phosphate radical precipitation).After pH is stable, carry out solid-liquid separation, will precipitate (being the phosphate radical precipitation) and reclaim, the hydrolysis after neutralization is further purified.
3. purifying:
Adopt anionite-exchange resin and Zeo-karb, the hydrolyzed solution after neutralization is carried out to purifying, obtain the hydrolyzed solution after purifying.
4. purifying elutriant phosphate radical precipitates.
The ion exchange resin used to purifying carries out wash-out regeneration, obtains elutriant.In elutriant, adding milk of lime adjusting pH is 9.0, obtains supernatant liquor and precipitation (being the phosphate radical precipitation).After pH is stable, carry out solid-liquid separation, will precipitate (being the phosphate radical precipitation) and reclaim.
5.D-the preparation of wood sugar, L-arabinose:
Hydrolyzed solution after purifying, through analog stream movable bed chromatographic separation, concentrated, crystallization, prepares D-wood sugar and L-arabinose crystal.
6. the phosphoric acid resource utilization recycles:
Add phosphoric acid to pH3.0 the precipitation of the phosphate radical in step 2 and step 4, until solid all dissolves, be precipitated lysate.
Detect the phosphoric acid value of resolution of precipitate liquid, after the allotment, join in sugarcane juice and carry out the resource utilization recycling according to actual needs.
Embodiment 2
The method operation steps that recycling phosphoric acid prepares D-wood sugar, L-arabinose is as follows:
1. raw material hydrolysis:
It is that 8.0% phosphoric acid is hydrolyzed that the sugarcane marrow adds mass percentage concentration, and the solid-to-liquid ratio kg/L of sugarcane marrow and phosphoric acid is 1:1, and hydrolysis temperature is 130 ℃, and hydrolysis time is 1h.
After being hydrolyzed, obtain hydrolysed mix, hydrolysed mix is filtered, obtain hydrolyzed solution.
2. the hydrolyzed solution phosphate radical precipitates:
In hydrolyzed solution, add milk of lime to carry out neutralization precipitation, regulate pH to 7.2, the hydrolyzed solution after being neutralized and precipitation (being the phosphate radical precipitation).After pH is stable, carry out solid-liquid separation, will precipitate (being the phosphate radical precipitation) and reclaim, the hydrolysis after neutralization is further purified.
3. purifying:
Adopt anionite-exchange resin and Zeo-karb, the hydrolyzed solution after neutralization is carried out to purifying, obtain the hydrolyzed solution after purifying;
4. purifying elutriant phosphate radical precipitates:
The ion exchange resin used to purifying carries out wash-out regeneration, obtains elutriant.In elutriant, adding milk of lime adjusting pH is 7.2, obtains supernatant liquor and precipitation (being the phosphate radical precipitation).After pH is stable, carry out solid-liquid separation, will precipitate (being the phosphate radical precipitation) and reclaim.
5.D-the preparation of wood sugar, L-arabinose:
Hydrolyzed solution after purifying, through analog stream movable bed chromatographic separation, concentrated, crystallization, prepares D-wood sugar and L-arabinose crystal.
6. the phosphoric acid resource utilization recycles:
Add sulfurous acid to pH4.5 the precipitation of the phosphate radical in step 2 and step 4, until solid all dissolves, be precipitated lysate.
Detect the phosphoric acid value of resolution of precipitate liquid, after the allotment, join in sugarcane juice and carry out the resource utilization recycling according to actual needs.
Embodiment 3
The method operation steps that recycling phosphoric acid prepares D-wood sugar, L-arabinose is as follows:
1. raw material hydrolysis:
It is that 5.0% phosphoric acid is hydrolyzed that Caulis Sacchari sinensis leaf adds mass percentage concentration, and the solid-to-liquid ratio kg/L of Caulis Sacchari sinensis leaf and phosphoric acid is 1:5, and hydrolysis temperature is 121 ℃, and hydrolysis time is 4h.
After being hydrolyzed, obtain hydrolysed mix, hydrolysed mix is filtered, obtain hydrolyzed solution.
2. the hydrolyzed solution phosphate radical precipitates:
In hydrolyzed solution, add milk of lime to carry out neutralization precipitation, regulate pH to 5.0, the hydrolyzed solution after being neutralized and precipitation (being the phosphate radical precipitation).After pH is stable, carry out solid-liquid separation, will precipitate (being the phosphate radical precipitation) and reclaim, the hydrolysis after neutralization is further purified.
3. purifying:
Adopt anionite-exchange resin and Zeo-karb, the hydrolyzed solution after neutralization is carried out to purifying, obtain the hydrolyzed solution after purifying.
4. purifying elutriant phosphate radical precipitates:
The ion exchange resin used to purifying carries out wash-out regeneration, obtains elutriant.In elutriant, adding milk of lime adjusting pH is 8.1, obtains supernatant liquor and precipitation (being the phosphate radical precipitation).After pH is stable, carry out solid-liquid separation, will precipitate (being the phosphate radical precipitation) and reclaim.
5.D-the preparation of wood sugar, L-arabinose:
Hydrolyzed solution after purifying, through analog stream movable bed chromatographic separation, concentrated, crystallization, prepares D-wood sugar and L-arabinose crystal.
6. the phosphoric acid resource utilization recycles:
The stove drying of phosphate radical in step 2 and step 4 precipitation, to pH3.5, until solid all dissolves, is precipitated to lysate.
Detect the phosphoric acid value of resolution of precipitate liquid, after the allotment, join in sugarcane juice and carry out the resource utilization recycling according to actual needs.
Embodiment 4
The method operation steps that recycling phosphoric acid prepares D-wood sugar, L-arabinose is as follows:
1. raw material hydrolysis:
It is that 6.0% phosphoric acid is hydrolyzed that bagasse adds mass percentage concentration, and the solid-to-liquid ratio kg/L of bagasse and phosphoric acid is 1:3, and hydrolysis temperature is 125 ℃, and hydrolysis time is 3h.
After being hydrolyzed, obtain hydrolysed mix, hydrolysed mix is filtered, obtain hydrolyzed solution.
2. the hydrolyzed solution phosphate radical precipitates:
In hydrolyzed solution, add milk of lime to carry out neutralization precipitation, regulate pH to 4.8, the hydrolyzed solution after being neutralized and precipitation (being the phosphate radical precipitation).After pH is stable, carry out solid-liquid separation, will precipitate (being the phosphate radical precipitation) and reclaim, the hydrolysis after neutralization is further purified.
3. purifying:
Adopt anionite-exchange resin and Zeo-karb, the hydrolyzed solution after neutralization is carried out to purifying, obtain the hydrolyzed solution after purifying.
4. purifying elutriant phosphate radical precipitates:
The ion exchange resin used to purifying carries out wash-out regeneration, obtains elutriant.In elutriant, adding milk of lime adjusting pH is 8.5, obtains supernatant liquor and precipitation (being the phosphate radical precipitation).After pH is stable, carry out solid-liquid separation, will precipitate (being the phosphate radical precipitation) and reclaim.
5.D-the preparation of wood sugar, L-arabinose:
Hydrolyzed solution after purifying, through analog stream movable bed chromatographic separation, concentrated, crystallization, prepares D-wood sugar and L-arabinose crystal;
6. the phosphoric acid resource utilization recycles:
Add phosphoric acid to pH3.0 the precipitation of the phosphate radical in step 2 and step 4, until solid all dissolves, be precipitated lysate.
Detect the phosphoric acid value of resolution of precipitate liquid, after the allotment, join in sugarcane juice and carry out the resource utilization recycling according to actual needs.
Claims (5)
1. a recycling phosphoric acid prepares the method for D-wood sugar, L-arabinose.It is characterized in that: method is by 1) the raw material hydrolysis; 2) hydrolyzed solution phosphate radical precipitation; 3) purifying; 4) purifying elutriant phosphate radical precipitation; 5) preparation of D-wood sugar, L-arabinose; 6) phosphoric acid resource utilization recycling operates, and concrete steps are as follows:
1) raw material hydrolysis:
It is that 3.0～8.0% phosphoric acid is hydrolyzed that bagasse, sugarcane marrow or Caulis Sacchari sinensis leaf add mass percentage concentration, and the solid-to-liquid ratio kg/L of bagasse, sugarcane marrow or Caulis Sacchari sinensis leaf weight and phosphoric acid volume is 1: 1～1: 10, and hydrolysis temperature is 110～130 ℃, and hydrolysis time is 1～5h; After being hydrolyzed, obtain hydrolysed mix, hydrolysed mix is filtered, obtain hydrolyzed solution;
2) hydrolyzed solution phosphate radical precipitation:
In hydrolyzed solution, add milk of lime to carry out neutralization precipitation, regulate pH to 4.5～7.2, after pH was stable, the hydrolyzed solution after being neutralized and phosphate radical precipitation, carried out solid-liquid separation, and the phosphate radical precipitation is reclaimed, and hydrolyzed solution is further purified;
3) purifying:
Adopt anionite-exchange resin and Zeo-karb, hydrolyzed solution is carried out to purifying, obtain the hydrolyzed solution after purifying;
4) purifying elutriant phosphate radical precipitation:
The ion exchange resin used to purifying carries out wash-out regeneration, obtains elutriant, and in elutriant, adding milk of lime adjusting pH is 7.2～9.0, after pH is stable, carries out solid-liquid separation, obtains supernatant liquor and phosphate radical precipitation, and the phosphate radical precipitation is reclaimed;
5) preparation of D-wood sugar, L-arabinose:
Hydrolyzed solution after purifying, through analog stream movable bed chromatographic separation, concentrated, crystallization, prepares D-wood sugar and L-arabinose crystal;
6) phosphoric acid resource utilization recycling:
By step 2) and step 4) in phosphate radical precipitation add phosphoric acid, sulfurous acid to pH3.0～4.5, until solid all dissolves, be precipitated lysate;
Detect the phosphoric acid value of resolution of precipitate liquid, after the allotment, join in sugarcane juice and carry out the resource utilization recycling according to actual needs.
2. recycling phosphoric acid as claimed in claim 1 prepares the method for D-wood sugar, L-arabinose, it is characterized in that: described recycling phosphoric acid is the phosphate radical resource reutilization, being hydrolyzed phosphate radical used is applied in the cane juice clarification technique of cane sugar manufacture after neutralization precipitation reclaims, phosphate radical is deposited in filter mud again, the filter mud as fertilizer sources utilizes again, realizes resource circulation utilization.
3. recycling phosphoric acid as claimed in claim 1 prepares the method for D-wood sugar, L-arabinose, it is characterized in that: described step 2) the hydrolyzed solution phosphate radical is precipitated as in hydrolyzed solution and adds milk of lime to carry out neutralization precipitation, regulate pH to 4.8～5.0, the hydrolyzed solution after being neutralized and phosphate radical precipitation.
4. recycling phosphoric acid as claimed in claim 1 prepares the method for D-wood sugar, L-arabinose, it is characterized in that: described step 4) the elutriant phosphate radical is precipitated as purifying ion exchange resin used is carried out to wash-out regeneration, obtains elutriant; In elutriant, adding milk of lime adjusting pH is 8.1, obtains supernatant liquor and phosphate radical precipitation.
5. recycling phosphoric acid as claimed in claim 1 prepares the method for D-wood sugar, L-arabinose, it is characterized in that: described step 6) phosphoric acid resource utilization recycling method is that the phosphate radical precipitation adds phosphoric acid, sulfurous acid, regulate pH to 3.0 solid is all dissolved, join in the sugarcane juice of cane sugar manufacture and carry out recycling.
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