CN108676820A - A kind of active xylitol and its manufacturing method using enzyme and microbial process manufacture - Google Patents
A kind of active xylitol and its manufacturing method using enzyme and microbial process manufacture Download PDFInfo
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Abstract
The invention discloses a kind of active xylitols and its manufacturing method using enzyme and microbial process manufacture, the activity xylitol is with 60 parts 70 parts clean by weight of discarded shaddock ped, clean 25 parts of 30 parts of the like waste of stalk are raw material, by mechanical pelleting, wash de-ash, lignoenzyme enzymolysis xylogen is polysaccharide, high-temperature acid environment hydrolyzes, alkalize compound marl, activated carbon once decolourizes to clean, phosphoric acid neutralizes, the inferior Dbaly yeast bacterium of the Chinese, which is cultivated, switches through microbial reaction and obtains the xylitol solution containing partial impurities, it is finally obtained using condensing crystallizing after activated carbon secondary decolourization removing impurity again.Manufacturing process of the present invention is simple, at low cost, with short production cycle, environmentally protective nuisanceless, active high easily absorption, purity are relatively high.
Description
Technical field
The present invention relates to acyclic or carbocyclic compound field more particularly to a kind of work using enzyme and microbial process manufacture
Property xylitol and its manufacturing method.
Background technology
Xylitol in currently available technology refers to originating in Finland, is from silver birch, Oak Tree, corncob, sugarcane
A kind of natural sweetener extracted in the plant materials such as slag.Presently commercially available xylitol is mainly by corncob, bagasse
Prepared by equal agricultural crops carry out deep processing is a kind of natural, health sweetener, for the body of people, xylose
Alcohol is nor one kind " thing from abroad ", it is originally the intermediate of the normal carbohydate metabolism of people's body, it is all sugar alcohol sweeteners
Middle maximum one kind of endothermic value, therefore when eating in solid form, it can pleasant refrigerant sense be generated in mouth.Xylitol it is not cariogenic and
There are anti-caries, metabolism is not adjusted by insulin, and complete in human body metabolism, calorific value 16.72kJ/g can be used as glycosuria
The heat energy of patient.But what the prior art mainly utilized is chemical extraction in agricultural product, produces that threshold is high, the production cycle is long, also
Certain pollution is will produce, while the anti-raw material used is also used as animal feed and is utilized in fact, there is certain economic valence
Value, therefore production cost is also higher, and product is finally made（Commercial product）Determination of Xylitol generally 50% or so, and it is pure
The xylitol absorption of human body efficiency of crops extraction is relatively low.
Activity xylitol in the prior art is limited to the missing of technical field and practical experience, the green in complete meaning
Environment-friendly active xylitol does not occur really also, therefore, production week simple, at low cost still without a kind of manufacturing process currently on the market
Phase is short, it is environmentally protective it is nuisanceless, active it is high easily absorb, the active xylitol that purity is relatively high.
Therefore it is simple, at low cost, with short production cycle, environmentally protective nuisanceless, active to be badly in need of a kind of manufacturing process in the market
The relatively high active xylitol of high easily absorption, purity.
Invention content
To solve drawbacks described above existing in the prior art, the present invention is intended to provide a kind of manufacturing process it is simple, it is at low cost,
The relatively high active xylitol of with short production cycle, environmentally protective nuisanceless, active high easily absorption, purity.
In order to achieve the above-mentioned object of the invention, the present invention uses following technical scheme：It is a kind of to use enzyme and microbial process system
The manufacturing method for the active xylitol made, includes the following steps：
1）Raw material prepare
1. raw material prepare：Prepare 60 parts -70 parts of clean discarded shaddock ped, 25 parts -30 parts clean of stalk, phosphinylidyne by weight
850 parts -1000 parts of the sulfuric acid of 3 parts -5 parts of amine, Solute mass fraction 1%, phosphate aqueous solution, the foot of enough Solute mass fractions 10%
Measure pulverized limestone, enough pure water, sufficient active charcoal；
2. decomposing activation auxiliary material to prepare：Prepare the inferior Dbaly yeast bacteria agent of enough Chinese, enough lignoenzyme aquas by weight；
3. equipment and tooling prepare：Preparing machine cutter device, the temperature control reaction for being provided with bottom ventilation device and agitating device
Kettle；
2）Xylose solution manufactures
1. by the stage 1）1. clean discarded shaddock ped and clean stalk that step prepares uses the stage 1）3. machine that step prepares
Tool cutter device is chopped into the particle of grain size 0.5mm-1mm, obtains raw material particle；
2. using the pure water raw material particle that repeatedly 1. 3 times -5 times rinse steps obtain, the particle that deashes is obtained；
3. the 2. particle that deashes that step obtains is immersed the stage 1）In 2. lignoenzyme aqua that step prepares, it is warming up to 25
DEG C -30 DEG C, 6h-8h is kept, obtains hemicellulose enzymolysis and polysaccharide mixed liquor；
4. 3. hemicellulose enzymolysis that step obtains and the heating of polysaccharide mixed liquor are concentrated into after 200 parts of parts by weight and the stage 1）Step
The sulfuric acid of the rapid Solute mass fraction 1% 1. prepared is mixed and stirred for uniformly, being warming up to 130 DEG C -140 DEG C, keeps 15min-
18min obtains acidolysis solution；
5. being gradually added into the stage 1 in 4. acidolysis solution that step obtains）1. pulverized limestone that step prepares, until pH value adjust to
10-11 obtains mixed solution；
6. being gradually added into the stage 1 in 5. mixed solution that step obtains）1. activated carbon that step prepares decolourizes completely to solution,
Then Solid content is detached, solution is retained, which is required xylose solution；
3）The manufacture of xylitol
1. in the stage 2）The stage 1 is slowly added dropwise in 6. xylose solution that step obtains）1. phosphoric acid solution that step prepares, until solution
PH value is reduced to 7-7.5, obtains neutralizer；
2. it is 170g/L-180g/L that 1. neutralizer heating that step obtains, which is concentrated into Xylose Content, substrate solution is obtained；
3. 2. substrate solution that step obtains is poured into the stage 1）In 3. temperature control reaction kettle that step prepares, then in reaction kettle
Implantation stage 1）The 2. inferior Dbaly yeast bacteria agent of the Chinese and stage 1 that step prepares）1. carbamide that step prepares, is warming up to 20
DEG C -25 DEG C, it is passed through enough air, and open and stir with 300rpm-500rpm, continues 3h-4h；35 DEG C -38 DEG C are then heated to,
It is slowly introducing air by the flow of 10ml/Ls-15ml/Ls with substrate solution stereometer, with the rate of 120rpm-150rpm
It is stirred, reacts 5h-6h, obtain xylitol solution；
4）Xylitol crystallizes
1. using activated carbon to the stage 3）3. xylitol solution that step obtains carries out decolorization again, then carries out solid-liquid point
From, then solution is heated and is concentrated into crystallization, which is required active xylitol.
Using the above method manufacture using enzyme and microbial process manufacture active xylitol, the activity xylitol be with
60 parts -70 parts clean of discarded shaddock ped, clean 25 parts of -30 parts of the like waste of stalk are raw material by weight, by machine
Tool is granulated, washing de-ash, lignoenzyme enzymolysis xylogen are polysaccharide, the hydrolysis of high-temperature acid environment, alkalize compound marl, work
Property charcoal once decolourize removal of impurities, phosphoric acid neutralizes, the inferior Dbaly yeast bacterium of the Chinese is cultivated and switches through microbial reaction and obtain miscellaneous containing part
The xylitol solution of matter, then finally obtained using condensing crystallizing after activated carbon secondary decolourization removing impurity.
Compared with prior art, by adopting the above-described technical solution, the present invention has the following advantages：（1）The present invention
In, no longer such as the method that the prior art destroys lignin using concentrated base, concentrated acid or high-temperature steam explosion treatment, but use machine
Tool is granulated refinement cooperation enzymolysis xylogen and will be detached as the hemicellulose of raw material, and reaction is mild thoroughly, production cost is low, together
When it is environmental friendly nuisanceless, security risk will not be caused.（2）Different from the prior art use concentration 98% the concentrated sulfuric acid into
The hydrolysis of hemicellulose of row bagasse, corn ear etc., the present invention promote former with shaddock ped and stalk only with dilute sulfuric acid cooperation high temperature
The hydrolysis of hemicellulose of material, this is because its fibre structure of material selected by the present invention and sugarcane selected in routine techniques
Slag, corn ear fibre structure and different, stability is relatively poor, on the other hand, since the raw material of the present invention is completely using useless
Gurry（Shaddock ped can not generally be recycled as feed etc., and crop straw burning has been prohibited for country, pollutes the environment）, raw
It produces at low cost and is conducive to environmental protection.（3）Different from the xylitol producing process of routine techniques, due to the shadow of a large amount of impurity after hydrolysis
It rings, microbial process can not be used（A large amount of products such as acetic acid, uronic acid, humic acid etc. of hydrolysis all have apparent antibacterial work
With the vital movement of microorganism can be inhibited）It is produced, the present invention is simply with lime（Main ingredient is calcium hydroxide）For work(
Energy agent, one side alkalizing solution destroy the activity of sour matter in solution, on the one hand utilize many organic acid calcium salts itself not soluble in water
The most of impurity of characteristic removal, purified solution, then by activated carbon adsorption solid and insoluble organic not soluble in water, into one
Step has purified solution, is laid the foundation for follow-up microbial reaction.（4）It is directly carried out after purification solution different from the prior art
Extraction, the present invention are first tentatively neutralized using phosphoric acid, are existed this is because producing the high microorganism of xylitol and being generally only suitable for existence
In neutral or acid solution, alkaline environment can inhibit its activity, meanwhile, phosphorus is also microorganism selected by the present invention --- Han Xunde
Important nutrient needed for Bali saccharomycete vital movement.（5）The inferior Dbaly yeast bacterium of the Chinese that the present invention especially selects is application
People's screening from multiple-microorganism after testing many times show that it is not the highest microorganism of per unit area yield xylitol, but
Extremely agree with the process route of the present invention, main cause is in the Pseudomonas facultative anaerobic bacteria, it is using carbamide as nitrogen source, oxygen
Gas is sufficient, 20 DEG C -25 DEG C（Room temperature）Temperature, a large amount of polysaccharide for decomposing of lignin it is existing under conditions of can quickly breed and big
Amount consumption polysaccharide（At this time due to lacking TCA approach media, which does not consume xylose substantially, and principle is probably similar to human body elder generation
Labile carbohydrate organic matter is consumed, post consumption needs the fat that enzyme coordinates）, microorganism species concentration is big after mass propagation
Width improves, while largely consuming the polysaccharide for being difficult to detach, and improves final product --- the purity of xylitol；And with phosphinylidyne
Amine is nitrogen source, micro- oxygen（Pay attention to it not being complete anaerobism at this time）、35℃-38℃（The production xylitol enzymatic activity highest of microorganism secretion）
Temperature, a large amount of xyloses it is existing under the conditions of, which stops breeding, by quickly and efficiently vital movement by xylose
At xylitol, simultaneously because not being complete anaerobic respiration, the speed for producing acid is unhappy（It mentions above, excessively high acid concentration meeting
Inhibit the vital activity of microorganism, and it is also to have carried out largely to obtain the amount for being passed through air needed for micro-oxygen conditions and stir speed (S.S.)
What verification experimental verification just obtained）, it is ensured that reaction more persistently, quickly, and realizes the technique of so sophisticated functions substantially only
It is to change the flow for being passed through air and slightly improve temperature, therefore this is science and the precise and tiny combination of microorganism,
It is the best match that applicant to microbiologic properties and process route obtain after repeatedly groping.（6）Different from existing skill
Xylitol is produced in art only once to purify, the present invention greatly improves the final purity for obtaining xylitol by purifying twice,
According to available data, for presently commercially available xylitol purity generally 50% or so, good patented technology can reach 60%, and of the invention
Secondarily purified again by microbial consumption polysaccharide, the xylitol purity of acquisition is 72%-74%, and more value object is spoken approvingly of, the present invention
Method xylitol yield be 82%-86%, be better than routine techniques 65%-75%.Therefore the present invention have manufacturing process it is simple, at
This relatively high characteristic of low, with short production cycle, environmentally protective nuisanceless, active high easily absorption, purity.
Specific implementation mode
Embodiment 1：
A kind of active xylitol using enzyme and microbial process manufacture, the activity xylitol are given up with clean by weight
Shaddock ped 60Kg, clean stalk 25Kg the like waste are abandoned for raw material, by mechanical pelleting, washing de-ash, lignoenzyme enzyme
Solution lignin, which is polysaccharide, high-temperature acid environment hydrolyzes, alkalize compound marl, activated carbon once decolourize cleans, phosphoric acid neutralizes, the Chinese
Inferior Dbaly yeast bacterium, which is cultivated, switches through microbial reaction and obtains the xylitol solution containing partial impurities, then uses activated carbon two
Secondary decoloration removes condensing crystallizing after impurity and finally obtains.
The above-mentioned manufacturing method using enzyme and the active xylitol of microbial process manufacture includes the following steps：
1）Raw material prepare
1. raw material prepare：Prepare clean discarded shaddock ped 60Kg, clean stalk 25Kg, carbamide 3Kg, solute by weight
The sulfuric acid 850Kg of mass fraction 1%, the phosphate aqueous solution of enough Solute mass fractions 10%, enough pulverized limestones, enough pure water,
Sufficient active charcoal；
2. decomposing activation auxiliary material to prepare：Prepare the inferior Dbaly yeast bacteria agent of enough Chinese, enough lignoenzyme aquas by weight；
3. equipment and tooling prepare：Preparing machine cutter device, the temperature control reaction for being provided with bottom ventilation device and agitating device
Kettle；
2）Xylose solution manufactures
1. by the stage 1）1. clean discarded shaddock ped and clean stalk that step prepares uses the stage 1）3. machine that step prepares
Tool cutter device is chopped into the particle of grain size 0.5mm-1mm, obtains raw material particle；
2. using the pure water raw material particle that repeatedly 1. 3 rinse steps obtain, the particle that deashes is obtained；
3. the 2. particle that deashes that step obtains is immersed the stage 1）In 2. lignoenzyme aqua that step prepares, it is warming up to 25
DEG C, 6h is kept, hemicellulose enzymolysis and polysaccharide mixed liquor are obtained；
4. 3. hemicellulose enzymolysis that step obtains and the heating of polysaccharide mixed liquor are concentrated into after parts by weight 200Kg and the stage 1）Step
The sulfuric acid of the rapid Solute mass fraction 1% 1. prepared is mixed and stirred for uniformly, being warming up to 130 DEG C, keeps 15min, it is molten to obtain acidolysis
Liquid；
5. being gradually added into the stage 1 in 4. acidolysis solution that step obtains）1. pulverized limestone that step prepares, until pH value adjust to
10, obtain mixed solution；
6. being gradually added into the stage 1 in 5. mixed solution that step obtains）1. activated carbon that step prepares decolourizes completely to solution,
Then Solid content is detached, solution is retained, which is required xylose solution；
3）The manufacture of xylitol
1. in the stage 2）The stage 1 is slowly added dropwise in 6. xylose solution that step obtains）1. phosphoric acid solution that step prepares, until solution
PH value is reduced to 7, obtains neutralizer；
2. it is 170g/L that 1. neutralizer heating that step obtains, which is concentrated into Xylose Content, substrate solution is obtained；
3. 2. substrate solution that step obtains is poured into the stage 1）In 3. temperature control reaction kettle that step prepares, then in reaction kettle
Implantation stage 1）The 2. inferior Dbaly yeast bacteria agent of the Chinese and stage 1 that step prepares）1. carbamide that step prepares, is warming up to 20
DEG C, it is passed through enough air, and open and stir with 300rpm, continues 3h；35 DEG C are then heated to, is pressed with substrate solution stereometer
The flow of 10ml/Ls is slowly introducing air, is stirred with the rate of 120rpm, reacts 5h, obtains xylitol solution；
4）Xylitol crystallizes
1. using activated carbon to the stage 3）3. xylitol solution that step obtains carries out decolorization again, then carries out solid-liquid point
From, then solution is heated and is concentrated into crystallization, which is required active xylitol.
The xylitol of the present embodiment production, yield 83%, purity 72%, absorptivity are better than commercially available xylitol.
Embodiment 2
It is whole consistent with embodiment 1, it is in place of difference：
A kind of active xylitol using enzyme and microbial process manufacture, the activity xylitol are given up with clean by weight
Shaddock ped 70Kg, clean stalk 30Kg the like waste are abandoned for raw material, by mechanical pelleting, washing de-ash, lignoenzyme enzyme
Solution lignin, which is polysaccharide, high-temperature acid environment hydrolyzes, alkalize compound marl, activated carbon once decolourize cleans, phosphoric acid neutralizes, the Chinese
Inferior Dbaly yeast bacterium, which is cultivated, switches through microbial reaction and obtains the xylitol solution containing partial impurities, then uses activated carbon two
Secondary decoloration removes condensing crystallizing after impurity and finally obtains.
The above-mentioned manufacturing method using enzyme and the active xylitol of microbial process manufacture includes the following steps：
1）Raw material prepare
1. raw material prepare：Prepare clean discarded shaddock ped 70Kg, clean stalk 30Kg, carbamide 5Kg, solute by weight
The sulfuric acid 1000Kg of mass fraction 1%, the phosphate aqueous solution of enough Solute mass fractions 10%, enough pulverized limestones, enough pure water,
Sufficient active charcoal；
2）Xylose solution manufactures
2. using the pure water raw material particle that repeatedly 1. 5 rinse steps obtain, the particle that deashes is obtained；
3. the 2. particle that deashes that step obtains is immersed the stage 1）In 2. lignoenzyme aqua that step prepares, it is warming up to 30
DEG C, 8h is kept, hemicellulose enzymolysis and polysaccharide mixed liquor are obtained；
4. 3. hemicellulose enzymolysis that step obtains and the heating of polysaccharide mixed liquor are concentrated into after parts by weight 200Kg and the stage 1）Step
The sulfuric acid of the rapid Solute mass fraction 1% 1. prepared is mixed and stirred for uniformly, being warming up to 140 DEG C, keeps 18min, it is molten to obtain acidolysis
Liquid；
5. being gradually added into the stage 1 in 4. acidolysis solution that step obtains）1. pulverized limestone that step prepares, until pH value adjust to
11, obtain mixed solution；
3）The manufacture of xylitol
1. in the stage 2）The stage 1 is slowly added dropwise in 6. xylose solution that step obtains）1. phosphoric acid solution that step prepares, until solution
PH value is reduced to 7.5, obtains neutralizer；
2. it is 180g/L that 1. neutralizer heating that step obtains, which is concentrated into Xylose Content, substrate solution is obtained；
3. 2. substrate solution that step obtains is poured into the stage 1）In 3. temperature control reaction kettle that step prepares, then in reaction kettle
Implantation stage 1）The 2. inferior Dbaly yeast bacteria agent of the Chinese and stage 1 that step prepares）1. carbamide that step prepares, is warming up to 25
DEG C, it is passed through enough air, and open and stir with 500rpm, continues 4h；38 DEG C are then heated to, is pressed with substrate solution stereometer
The flow of 15ml/Ls is slowly introducing air, is stirred with the rate of 150rpm, reacts 6h, obtains xylitol solution；
The xylitol of the present embodiment production, yield 86%, purity 74%, absorptivity are better than commercially available xylitol.
The foregoing description of the disclosed embodiments, only for enabling professional and technical personnel in the field to realize or using this hair
It is bright.Various modifications to these embodiments will be apparent to those skilled in the art, and determine herein
The General Principle of justice can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, originally
Invention is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein
Consistent widest range.
Claims (2)
1. a kind of manufacturing method using enzyme and the active xylitol of microbial process manufacture, it is characterised in that including following step
Suddenly：
1）Raw material prepare
1. raw material prepare：Prepare 60 parts -70 parts of clean discarded shaddock ped, 25 parts -30 parts clean of stalk, phosphinylidyne by weight
850 parts -1000 parts of the sulfuric acid of 3 parts -5 parts of amine, Solute mass fraction 1%, phosphate aqueous solution, the foot of enough Solute mass fractions 10%
Measure pulverized limestone, enough pure water, sufficient active charcoal；
2. decomposing activation auxiliary material to prepare：Prepare the inferior Dbaly yeast bacteria agent of enough Chinese, enough lignoenzyme aquas by weight；
3. equipment and tooling prepare：Preparing machine cutter device, the temperature control reaction for being provided with bottom ventilation device and agitating device
Kettle；
2）Xylose solution manufactures
1. by the stage 1）1. clean discarded shaddock ped and clean stalk that step prepares uses the stage 1）3. machine that step prepares
Tool cutter device is chopped into the particle of grain size 0.5mm-1mm, obtains raw material particle；
2. using the pure water raw material particle that repeatedly 1. 3 times -5 times rinse steps obtain, the particle that deashes is obtained；
3. the 2. particle that deashes that step obtains is immersed the stage 1）In 2. lignoenzyme aqua that step prepares, it is warming up to 25
DEG C -30 DEG C, 6h-8h is kept, obtains hemicellulose enzymolysis and polysaccharide mixed liquor；
4. 3. hemicellulose enzymolysis that step obtains and the heating of polysaccharide mixed liquor are concentrated into after 200 parts of parts by weight and the stage 1）Step
The sulfuric acid of the rapid Solute mass fraction 1% 1. prepared is mixed and stirred for uniformly, being warming up to 130 DEG C -140 DEG C, keeps 15min-
18min obtains acidolysis solution；
5. being gradually added into the stage 1 in 4. acidolysis solution that step obtains）1. pulverized limestone that step prepares, until pH value adjust to
10-11 obtains mixed solution；
6. being gradually added into the stage 1 in 5. mixed solution that step obtains）1. activated carbon that step prepares decolourizes completely to solution,
Then Solid content is detached, solution is retained, which is required xylose solution；
3）The manufacture of xylitol
1. in the stage 2）The stage 1 is slowly added dropwise in 6. xylose solution that step obtains）1. phosphoric acid solution that step prepares, until solution
PH value is reduced to 7-7.5, obtains neutralizer；
2. it is 170g/L-180g/L that 1. neutralizer heating that step obtains, which is concentrated into Xylose Content, substrate solution is obtained；
3. 2. substrate solution that step obtains is poured into the stage 1）In 3. temperature control reaction kettle that step prepares, then in reaction kettle
Implantation stage 1）The 2. inferior Dbaly yeast bacteria agent of the Chinese and stage 1 that step prepares）1. carbamide that step prepares, is warming up to 20
DEG C -25 DEG C, it is passed through enough air, and open and stir with 300rpm-500rpm, continues 3h-4h；35 DEG C -38 DEG C are then heated to,
It is slowly introducing air by the flow of 10ml/Ls-15ml/Ls with substrate solution stereometer, with the rate of 120rpm-150rpm
It is stirred, reacts 5h-6h, obtain xylitol solution；
4）Xylitol crystallizes
1. using activated carbon to the stage 3）3. xylitol solution that step obtains carries out decolorization again, then carries out solid-liquid point
From, then solution is heated and is concentrated into crystallization, which is required active xylitol.
2. using the active xylitol using enzyme and microbial process manufacture of claim 1 the method manufacture, feature exists
In：The activity xylitol is useless with 60 parts -70 parts clean by weight of discarded shaddock ped, 25 parts -30 parts clean of stalk etc.
Gurry is raw material, by mechanical pelleting, washing de-ash, lignoenzyme enzymolysis xylogen be polysaccharide, high-temperature acid environment hydrolysis,
Alkalize compound marl, activated carbon once decolourizes that removal of impurities, phosphoric acid neutralize, the inferior Dbaly yeast bacterium of the Chinese cultivates that switch through microorganism anti-
It answers and obtains the xylitol solution containing partial impurities, then is final using condensing crystallizing after activated carbon secondary decolourization removing impurity
It obtains.
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