CN106191328A

CN106191328A - A kind of xylose production process

Info

Publication number: CN106191328A
Application number: CN201610843912.4A
Authority: CN
Inventors: 邵荣珠
Original assignee: Individual
Current assignee: Individual
Priority date: 2016-09-23
Filing date: 2016-09-23
Publication date: 2016-12-07

Abstract

A kind of xylose production process, utilize corn cob as raw material, sequentially through include steam explosion, hydrochloric acid hydrolysis, solid-liquid separation, decolouring neutralization, ultra-filtration filters, electrodialysis desalination, low pressure reverse osmosis membrance concentration, the concentration of middle pressure reverse osmosis membrane, MVR evaporation and concentration, chromatographic refining desalination purification, ion exchange resin refine, concentrate, crystallize, be centrifuged, dry including step, finally give xylose product.The present invention reduces the energy consumption in xylose production, decreases pollution.

Description

A kind of xylose production process

Technical field

The present invention relates to technical field of xylose production, particularly relate to a kind of low power consuming, oligosaprobic xylose production process.

Background technology

Xylose is white crystals body sweeting agent, and sugariness is equivalent to the 70% of sucrose, it is impossible to provide heat for human body, but to people Bacillus bifidus in body intestinal has higher increment effect.The microecological environment of human body can be improved, improve immunity of organisms.? The aspects such as food processing, beverage are added, prepared by pet food are widely used, and are alternatively arranged as the wind of meat product, cereal product Improving agent and prepare meat flavoring, the raw material of high-grade color of soy sauce.The quality of life improving people there is critical function And effect.

It is with agricultural wastes such as corn cobs as raw material that traditional handicraft prepares xylose product, preprocessed remove impurity, sulphuric acid water Solution, calcium carbonate neutralization, activated carbon decolorizing, primary ions exchange purification, flush distillation concentration, Two-step ion-exchanging purification, secondary Evaporation and concentration, single effect evaporation, crystallize, be centrifuged, dry, sieve, the operation such as packaging is prepared from.

This technique and for example descends shortcoming:

1, owing to using sulphuric acid hydrolysis technique, containing substantial amounts of sulfate ion in xylose hydrolysis fluid, N-process carries again Enter substantial amounts of calcium ion, follow-up ion-exchange process is brought the biggest burden；Sulphuric acid hydrolysis makes hydrolyzed solution color very deep, Cause the biggest difficulty to later stage decolouring, and consume substantial amounts of activated carbon；In the waste water of sulphuric acid hydrolysis technique discharge, due to sulfate radical A large amount of existence, it is impossible to using anaerobic technique, its waste water processes cannot be up to standard；Owing to the chemism of sulphuric acid is low, institute during hydrolysis Consumption is the highest, gives the biggest load of desalination increase after hydrolysis, and it is from handing over load the highest with decolouring load.

2, traditional handicraft uses the vertical hydrolysis kettle of liner ceramic tile, and ceramic tile easily comes off, and tile binding material is corrosion-resistant Property is poor.And manufacturing process is complicated, can only do liner in scene, difficult in maintenance.

3, the refining and edulcoration of Xylose uses ion-exchange-resin process, when regenerating these anion and cation exchange resin Substantial amounts of spent acid, spent lye can be produced, cause wastewater discharge big, pollute environment serious.

4, concentration process uses high-pressure saturated steam that the Xylose of low concentration is concentrated into the xylose cream of high concentration all the time, steams Steam consumption is big.

As can be seen here, traditional method for producing xylose also exists the three-hypers problems such as high consumption, highly energy-consuming, high pollution, is not inconsistent Close national industrial policies requirement, there is bigger industry development risk.

Therefore, develop a kind of new xylose production process, not only there is urgent researching value, it may have good economy Benefit and commercial Application potentiality, this power place that present invention is accomplished just and basis.

Summary of the invention

In order to overcome the defect of prior art as indicated above, this is conducted in-depth research by the present inventor, is paying After a large amount of creative works, thus complete the present invention.

Specifically, the technical problem to be solved is: provide a kind of xylose production process, to solve Traditional Wood Sugar produces high energy consumption, the technical problem of high pollution.

For solving above-mentioned technical problem, the technical scheme is that

A kind of xylose production process, utilizes corn cob as raw material, sequentially passes through and include that steam explosion, hydrochloric acid hydrolyze, admittedly Liquid separation, decolouring neutralization, ultra-filtration filters, electrodialysis desalination, low pressure reverse osmosis membrance concentration, the concentration of middle pressure reverse osmosis membrane, MVR evaporation Concentrate, chromatographic refining desalination purifies, ion exchange resin refines, concentrates, crystallizes, is centrifuged, dries in interior step, finally gives Xylose product.

As further improving, a kind of xylose production process, comprise the steps:

S1, pre-treatment: take corn cob as raw material, first selecting crude drugs with winnower process, and then utilize roller screen to process, finally carry out clear water Clean；

Utilize selecting crude drugs with winnower can remove the light impurities such as the Stigma Maydis in corn cob, leaves, plastic bag, remove Semen Maydis with roller screen The big ratio heavy seeds such as dust in core, masonry, niblet, recycling clean water falls in corn cob the impurity such as the dust of remaining；

S2, Steam explosion pretreatment: the corn cob through the pre-treatment of step S1 is sprayed hydrochloric acid, imports the most heated vapour In blast chamber, it is passed through saturated vapor and material is heated by air, under uniform temperature and pressure, after maintaining certain time, wink Between pressure release；

Making hemicellulose in corn cob, lignin, cellulose separately, hemicellulose degradation is that oligosaccharide is (the most oligomeric The eleventh of the twelve Earthly Branches sugar)；Lignin active group increase and with cellulose from structure loosen separate, make cellulose crystallity strengthen, be refined Xylose creates condition；For utilizing hydrolysis slag to manufacture green glue-free environment friendly artificial board material to create condition.

S3, low temperature hydrochloric acid hydrolyze: the corn cob (moisture content 30%) through step S2 Steam explosion pretreatment is imported water In solution equipment, adding the hydrochloric acid solution of 0.2 0.4wt%, then pass to steam, be warming up to 100-105 DEG C and stop steam, pressure is 0.1-0.15Mpa, is incubated 12 hours, obtains being mixed with the hydrolysis melt cinder of hydrolyzed solution；

Wherein, the hydrochloric acid solution of 0.2 0.4wt% can use solid hydrolysis wash heat liquid configuration；

Corn cob material dry weight is 1:(2 4 with the weight ratio of the hydrochloric acid solution of 0.2 0.4wt%).

The hemicellulose in corn cob and the oligosaccharide degraded is made to be fully converted into xylose molecule.Dedicated water used The steel lining plastic reactor that solution equipment is produced by Cixi red plastic containers company limited.

S4, solid-liquid separation: the hydrolysis melt cinder being mixed with hydrolyzed solution step S3 obtained sends into press type solid-liquid separation dress Putting or carry out in gasbag-type equipment for separating liquid from solid solid-liquid separation, isolated xylose hydrolysis fluid, xylose hydrolysis fluid enters hydrolyzed solution Storage tank, carries out the refinement treatment of next procedure；

The solid hydrolysis residue obtained after separation is carried out, and cleanout fluid reclaims, for the hydrochloric acid solution in configuration step S3, New quick-fried broken corn cob is hydrolyzed, to reclaim residual sugar, to save water resource.

The solid hydrolysis residue once purged feeding fermentation tank obtained after separation carries out solid fermentation, and lignin is carried out the degree of depth Activation, creates conditions for being not added with any adhesive compacting environmental protection artificial board.

S5, decolouring neutralize: xylose hydrolysis fluid step S4 obtained, and are delivered to decolouring with acid-proof pump from hydrolyzed solution storage tank In post, activated carbon or macropore decolorizing resin is utilized to be gone by the impurity such as the pigment in xylose hydrolysis fluid, ash, colloid, visible slag stain Remove so that it is light transmittance reaches 20 50%, and add appropriate NaOH and be adjusted to save PH to 2.5-3.5, obtain transparent xylose and take off Color liquid；

S6, ultra-filtration filters: Decoloration of Xylose liquid step S5 obtained, utilize the semi permeability characteristic of ultrafilter membrane, selects molecule Amount is 20000 daltonian clean star ultrafilter membranes, separates molecular weight more than 20000 daltonian all impurity and pigment, Obtain the Xylose of clarification, process for follow-up film and create conditions；

Device therefor is the Full-automatic ultra-filtering device that Weifang Jie Xing Water Management Equipment Ltd. produces.

S7, electrodialysis desalination: Xylose step S6 obtained, utilize the nonconducting characteristic of Xylose itself, at direct current Under the effect of electric field, salt and the zwitterion of hydrolytic process generation that N-process produces are gone through anode membrane and cavity block respectively Remove, obtain the Xylose based on xylose and water.

The Xylose electrical conductivity obtained through electrodialysis desalination is reduced to about 1000us/cm by 10000us/cm.

The zwitterion that this process will be removed in 80-90% hydrolyzed solution, exchanges refined for follow-up chromatographic refining and ion Reduce burden, decrease the discharge of spent acid alkali.

Device therefor is the continuous electrodialysis desalination device that Weifang Jie Xing Water Management Equipment Ltd. produces.

S8, low pressure reverse osmosis membrance concentration: Xylose step S7 obtained is pressurized to 1.5-2.0Mpa, through molecular weight be 100 daltonian low-pressure reverse osmosis membranes, molecular weight is that 150 daltonian xyloses are trapped, less than the salt of 100 Dalton molecular weights Divide and water is through film, obtain concentration and reach the Xylose of 10wt%.

This step reaches low-pressure energy-saving and concentrates the purpose of Xylose.Concentration reaches the Xylose of 10% and goes next procedure, thoroughly The water crossed does hydrolysis dosing water, is greatly saved energy consumption, saves water resource.

Device therefor is the Full-automatic reverse-osmosis material concentration device that Weifang Jie Xing Water Management Equipment Ltd. produces.

S9, middle pressure reverse osmosis membrane concentrate: concentration step S8 obtained reaches the Xylose of 10wt% and is pressurized to 3-7Mpa, Entrance is pressed reverse osmosis membrane, the most automatically adjusts pressure and carry out secondary concentration, obtain concentration and reach the wood of 20wt% Sugar liquid；

In this step, concentration reaches the Xylose of 20wt% and is delivered to next procedure, and permeate does hydrolysis dosing water.

This process expense through water per ton is about 10 yuan, compared with the expense of equal 70 yuan of triple effect evaporation level per ton, often Ton water saves 60 yuan, and the high-quality pure water reclaimed can supplementing directly as tap water.

Device therefor be Weifang Jie Xing Water Management Equipment Ltd. produce automatically permeate material concentration device.

S10, MVR evaporation and concentration: concentration step S9 obtained reaches the Xylose of 20wt% and is heated to 60 DEG C, uses Xylose is evaporated concentrating by MVR vaporizer (i.e. mechanical steam recompression vaporizer), and obtaining concentration is 40 50wt% Xylose；

During heating, the heat produced when using the hydrolysis of step S3.

The heat produced due to water in advance solution makes Xylose be warmed to 60 DEG C, and whole evaporation process does not consume raw steam. The power consumption evaporating water per ton is 20-50KW, effectively reduces evaporation expense.

MVR vaporizer is different from common single-action falling liquid film or multiple-effect falling film vaporizer, and MVR is monomer evaporator, collection multiple-effect fall Film evaporator, takes stagewise to evaporate according to required product concentration difference, i.e. product for the first time after effect body not When can reach desired concn, product is taken out by effect external body pipeline after leaving effect body by product by the vacuum pump of effect body bottom To effect body top again by effect body, then by this effect body that iterates through to reach desired concn.Imitate internal portion for arrangement Tubule, pipe is internal be product, and outside is steam, makes due to the increase of pipe inner area in product flow process from top to bottom Product is membranaceous flowing, to increase heating surface area, is imitating internal formation negative pressure by vacuum pump, is reducing the boiling point of water in product, Thus reach to concentrate, product evaporating temperature is about 60 DEG C.

S11, chromatographic refining desalination purify: concentration step S10 obtained is the Xylose of 40 50wt%, control temperature For 50-70 DEG C, use chromatographic isolation adsorbent resin to carry out refined desalination and purify, collect extract；

The suction to impurity such as the glucides such as xylose and calcium, magnesium, sodium, chlorine, nitrate anion and pigments of the chromatographic isolation adsorbent resin Attached coefficient is different, and the time causing various material outflow system is the most different, and the component first flowed out (i.e. contains the sugar such as xylose extract The component that class material is more), the rear component flowed out, raffinate (the most impure more component), is collected extract respectively and carries Remaining liquid, extract carries out follow-up xylose preparation and processes, and after raffinate is concentrated, the side-product as xylose is sold；

S12, ion exchange resin are refined: extract step S11 obtained is exchanged by the ion equipped with anions and canons The ion exchange column that resin is composed in series, carries out further refinement treatment to Xylose, with remove its yin, yang contained from Son, obtains the electrical conductivity Xylose less than 5us/cm；

S13, concentrate, crystallize, be centrifuged, dry: the Xylose that step S12 is obtained, then use MVR vaporizer and the most single Single-effect evaporator is concentrated into the concentration of 81-84wt%, the mode of recycling evaporative crystallization to xylose refined liquid, makes xylose massecuite by not Saturated solution becomes saturated solution and is then converted to supersaturated solution, and its xylose crystal grain is constantly grown up and separates out, then by flat Xylose crystals is separated by centrifuge with mother solution, respectively obtains xylose crystals and xylose mother liquid, and xylose crystals passes through vibrated fluidized bed Xylose crystals is dried, obtains crystalline xylose finished product；Xylose mother liquid is sold as side-product.

As the preferred technical scheme of one, present invention additionally comprises the process step to waste water: use anaerobism, hydrolysis acid Change, aerobic, precipitation, light electrolysis, Fenton reagent, flocculation sediment carry out pretreatment, and mud is extruded by pressure filter, is delivered to organic Fertile production line；Waste water reaches the inflow requirement of follow-up equipment, then uses secondary filter, ultrafiltration, nanofiltration, reverse osmosis advanced process After, through water fully recovering to production line；Condensed water is delivered to the explosion of fodder production line and sprays saline in advance thus realize waste water Recycle.

As the preferred technical scheme of one, in step S2, the corn cob of hydrochloric acid will be sprayed with at steam explosion equipment Steam explosion intracavity utilizes saturated vapor and air to be heated to 120 DEG C, reaches pressure 1.1-1.5Mpa, pressurize 8-10 minute, then moment When decompression is spurted, producing indirect steam, raw material volume surges, and is acted on by mechanical force, and its solid material is destructurized.

As the preferred technical scheme of one, steam explosion equipment of the present invention (model is QB1500-3), refer to The steam explosion equipment of commercially available Chinese Academy of Sciences's process engineering institute invention, can crush material the moment of 0.00785 second.When So, it would however also be possible to employ other steam explosion equipment similar, that required effect can be reached.

As the preferred technical scheme of one, in step S3, low temperature hydrolysis process of the present invention, is special in the present invention Steel lining plastic reactor in complete, its temperature, pressure controllable, temperature controls as 100-105 DEG C., pressure is 0.1- 0.15Mpa, the response time is 1-2 hour, can be adjusted as required.Special steel lining plastic reactor is by the red plastics of Cixi Container company limited produces.

As the preferred technical scheme of one, in step S4, equipment for separating liquid from solid is used to carry out solid-liquid separation, described solid-liquid Segregation apparatus uses the one in Atmosphere Presser or hydraulic squeezing press.

Atmosphere Presser or hydraulic squeezing press compared to traditional flame filter press or centrifuge, have separating pressure high, Separation efficiency advantages of higher, can fully reclaim the xylose hydrolysis fluid in hydrolysis residue, it is ensured that higher hydrolysis yield.

As the preferred technical scheme of one, in step S7, using electrodialysis plant to complete, described electrodialysis plant uses One in heterogeneous ion-exchange membrane or homogeneous ion-exchange membrane, the DC voltage control of described electrodialysis plant is at 80-220V.

Described electrodialysis plant is produced by Weifang Jie Xing Water Management Equipment Ltd..

As the preferred technical scheme of one, in step S8, described low-pressure reverse osmosis membrane uses polyamide material antipollution Film, operating pressure is 1.5-2.0MPa.

As the preferred technical scheme of one, in step S9, medium pressure reverse osmosis membrane polyamide material pollution-resistant membrane, fortune Row pressure is 3.0-7.0MPa.

Low pressure of the present invention, middle pressure reverse osmosis membrane concentrator, be by Weifang Jie Xing Water Management Equipment Ltd. Produce.

As the preferred technical scheme of one, in step S11, described chromatographic isolation adsorbent resin uses calcium type chromatographic isolation Adsorbent resin, temperature range of operation is 50-70 DEG C.

Spent lye, waste hydrochloric acid liquor that anion and cation exchange resin of the present invention regeneration produces individually are deposited, in order to protect Card regenerated liquid and the quality of hydrolyzed solution, do not carry out reuse.Acid pickle is applied to waste water and processes the PH tune of light electrolysis and Fenton operation Joint, spent lye is applied to the pH value readjustment of flocculation sediment operation.

Waste water of the present invention processes, and pretreatment uses traditional anaerobism, hydrolysis acidification, aerobic and light electrolysis, Fenton The technology that reagent combines, it is ensured that pretreated waste water reaches the inflow requirement that successive depths processes.

Waste water of the present invention processes, and advanced treating used by surpassing that Weifang Jie Xing Water Management Equipment Ltd. provides The technology such as filter, nanofiltration, reverse osmosis, it is ensured that waste water is accomplished to recycle, and makes the water consumption of xylose production process be negligible.

After have employed technique scheme, the invention has the beneficial effects as follows:

1, use steam explosion technology that corn cob is carried out pretreatment, lignin, hemicellulose, cellulose separately, i.e. Simply hemicellulose is become oligoxylans, again lignin and cellulose separated and enhance respective characteristic, for rear Continuous environmental protection glue-free compacting artificial board creates condition, and production efficiency greatly improves again.

2, use the steel lining plastic reactor that the present invention is special, solve the etching problem of hydrochloric acid hydrolysis, manufacture, transport, tie up Protect the simplest.

3, using hydrochloric acid hydrolysis process, under same degree of hydrolysis, the chemical equivalent of hydrochloric acid has only to sulphuric acid equivalent 60%, so rear desalting refinement process load can reduce 40%, and the color of the xylose hydrolysis fluid of gained is shallower, and decolorising agent consumption is extremely 40% can be reduced less.

4, there is not the inhibitory action to anaerobe due to hydrochloric acid, so the waste water ratio tradition xylose that present invention process produces The effect that the waste water of production technology processes to be got well.

5, using NaOH to neutralize, make the composition increased in hydrolyzed solution single, follow-up electrodialysis desalination processes.

6, use ultra-filtration filters hydrolyzed solution, utilize the selective penetrated property of ultrafilter membrane, separate pigment and the impurity of macromole, clear Clear hydrolyzed solution, processes for refined xylose liquid and next step embrane method and creates conditions.

7, use electrodialysis desalination, utilize the nonconducting principle of Xylose, the various salinities in hydrolyzed solution are separated, desalination Rate, up to 80-90%, reduces the consumption of ion-exchange process soda acid, decreases the outfit expense of ion-exchange unit.

8, use low pressure reverse osmosis concentrating hydrolysate, by extremely low energy consumption (1 yuan/ton of water), hydrolyzed solution concentration is brought up to 10%.

9, press reverse osmosis concentration hydrolyzed solution in using, by relatively low energy consumption (3 yuan/ton of water), hydrolyzed solution concentration is brought up to 20%.Greatly reduce concentration expense.

10, use MVR concentration technique, utilize the steam coming from hydrolysing step generation to heat, steam need not be given birth to, only Just can evaporate one ton of water with the power consumption of 20-50KW, reduce evaporation expense.

11, use chromatographic separation technology to replace traditional ion exchange resin to refine purifying xylose liquid, do not consume soda acid, nothing The advantages such as regenerating spent acid aqueous alkali produces, and has separation efficiency high, and water consumption is few, and wastewater discharge is few, have the most energy-conservation, joint Water effect.

12, waste water of the present invention processes the waste water zero-discharge technology using Weifang Jie Xing Water Management Equipment Ltd. to provide, After preprocessed, advanced treating, wastewater to reach standard fully recovering；Mud is as the raw material producing fertilizer；Concentrate saline as raising The material pre-hydrojet of production resettlement.

12, the preparation method of the present invention is compared to the Technology of tradition xylose production, reduces the production cost of xylose, Improve the quality of xylose, waste water has been accomplished to recycle, and has significant economy, environment protecting.

In sum, the xylose production process that the present invention provides, it is possible to the effective ingredient in corn cob is fully discharged, carries The high output capacity of xylose, meanwhile, recycles follow-up particular step and has accomplished low energy consumption, low stain, and production technology is as one The flow process of individual entirety, mutually restricts between each step, collaborative, jointly achieves high yield, low energy consumption, oligosaprobic useful Effect, has and the most significantly improves.

Detailed description of the invention

Below in conjunction with specific embodiment, the present invention is further described.But the purposes of these exemplary embodiments and mesh Be only used for enumerate the present invention, not the real protection scope of the present invention is constituted any type of any restriction, more non-incite somebody to action this The protection domain of invention is confined to this.

Embodiment 1

A kind of xylose production process, comprises the steps:

S1, pre-treatment: take corn cob as raw material, first selecting crude drugs with winnower process, and then utilize roller screen to process, finally carry out clear water Clean；Utilize selecting crude drugs with winnower can remove the light impurities such as the Stigma Maydis in corn cob, leaves, plastic bag, remove corn cob with roller screen In dust, masonry, the big ratio heavy seeds such as niblet, recycling clean water falls in corn cob the impurity such as the dust of remaining；

S2, Steam explosion pretreatment: the corn cob through the pre-treatment of step S1 is sprayed hydrochloric acid, imports the most heated vapour In blast chamber, it is passed through saturated vapor and material is heated by air, under uniform temperature and pressure, after maintaining certain time, wink Between pressure release；Making hemicellulose in corn cob, lignin, cellulose separately, hemicellulose degradation is oligosaccharide (the most oligomeric the eleventh of the twelve Earthly Branches Sugar)；Lignin active group increase and with cellulose from structure loosen separate, make cellulose crystallity strengthen, for refined wood Sugar creates condition；For utilizing hydrolysis slag to manufacture green glue-free environment friendly artificial board material to create condition.

Concrete steam explosion step is: utilized at the steam explosion intracavity of steam explosion equipment by the corn cob being sprayed with hydrochloric acid Saturated vapor and air are heated to 120 DEG C, reach pressure 1.1Mpa, pressurize 8 minutes, then when instant decompression is spurted, produce secondary Steam, raw material volume surges, and is acted on by mechanical force, and its solid material is destructurized.Steam explosion of the present invention sets Standby (model is QB1500-3), refers to the steam explosion equipment of commercially available Chinese Academy of Sciences's process engineering institute invention, can be Material is crushed by the moment of 0.00785 second.It is of course also possible to use other steam similar, that required effect can be reached Blasting gear.

S3, low temperature hydrochloric acid hydrolyze: the corn cob (moisture content 30%) through step S2 Steam explosion pretreatment is imported water In solution equipment, adding the hydrochloric acid solution of 0.2wt%, then pass to steam, be warming up to 100 DEG C and stop steam, pressure is 0.1Mpa, protects Temperature 1 hour, obtains being mixed with the hydrolysis melt cinder of hydrolyzed solution；Wherein, the hydrochloric acid solution of 0.2wt% can use solid to hydrolyze wash heat Liquid configures；Corn cob material dry weight is 1:2 with the weight ratio of the hydrochloric acid solution of 0.2wt%.This step makes in corn cob half Cellulose and the oligosaccharide degraded are fully converted into xylose molecule.Special hydrolytic equipment used is held by the red plastics of Cixi The steel lining plastic reactor that device company limited produces, steel lining plastic reactor temperature, pressure controllable, it is 100 DEG C that temperature controls, pressure For 0.1Mpa, the response time is 1 hour, can be adjusted as required.

S4, solid-liquid separation: the hydrolysis melt cinder being mixed with hydrolyzed solution step S3 obtained is sent in equipment for separating liquid from solid Row solid-liquid separation, isolated xylose hydrolysis fluid, xylose hydrolysis fluid enters hydrolyzed solution storage tank, carries out the refined place of next procedure Reason；The solid hydrolysis residue obtained after separation is carried out, and cleanout fluid reclaims, for the hydrochloric acid solution in configuration step S3, to newly Quick-fried broken corn cob is hydrolyzed, to reclaim residual sugar, to save water resource.The once purged feeding of solid hydrolysis residue obtained after separation is sent out Ferment tank carries out solid fermentation, and lignin is carried out deep activation, for being not added with any adhesive compacting environmental protection artificial board wound Make condition.

In this step, using equipment for separating liquid from solid to carry out solid-liquid separation, described equipment for separating liquid from solid uses Atmosphere Presser Or the one in hydraulic squeezing press.Atmosphere Presser or hydraulic squeezing press are compared to traditional flame filter press or centrifuge, tool There are separating pressure height, separation efficiency advantages of higher, can fully reclaim the xylose hydrolysis fluid in hydrolysis residue, it is ensured that higher hydrolysis Yield.

S5, decolouring neutralize: xylose hydrolysis fluid step S4 obtained, and are delivered to decolouring with acid-proof pump from hydrolyzed solution storage tank In post, activated carbon or macropore decolorizing resin is utilized to be gone by the impurity such as the pigment in xylose hydrolysis fluid, ash, colloid, visible slag stain Remove so that it is light transmittance reaches 20%, and add appropriate NaOH and be adjusted to save PH to 2.5, obtain transparent Decoloration of Xylose liquid；

S6, ultra-filtration filters: Decoloration of Xylose liquid step S5 obtained, utilize the semi permeability characteristic of ultrafilter membrane, selects molecule Amount is 20000 daltonian clean star ultrafilter membranes, separates molecular weight more than 20000 daltonian all impurity and pigment, Obtain the Xylose of clarification, process for follow-up film and create conditions；Device therefor is Weifang Jie Xing Water Management Equipment Ltd. The Full-automatic ultra-filtering device produced.

S7, electrodialysis desalination: Xylose step S6 obtained, utilize the nonconducting characteristic of Xylose itself, at direct current Under the effect of electric field, salt and the zwitterion of hydrolytic process generation that N-process produces are gone through anode membrane and cavity block respectively Remove, obtain the Xylose based on xylose and water；The Xylose electrical conductivity obtained through electrodialysis desalination is dropped by 10000us/cm As little as about 1000us/cm；This process will remove the zwitterion in 80-90% hydrolyzed solution, for follow-up chromatographic refining and from Son exchange is refined reduces burden, decreases the discharge of spent acid alkali.This step uses electrodialysis plant to complete, and described electrodialysis fills Putting the one used in heterogeneous ion-exchange membrane or homogeneous ion-exchange membrane, the DC voltage control of described electrodialysis plant exists 80-220V.Described electrodialysis plant is produced by Weifang Jie Xing Water Management Equipment Ltd..

S8, low pressure reverse osmosis membrance concentration: Xylose step S7 obtained is pressurized to 1.5Mpa, be 100 through molecular weight Daltonian low-pressure reverse osmosis membrane, described low-pressure reverse osmosis membrane uses polyamide material pollution-resistant membrane, and operating pressure is 1.5MPa, Molecular weight is that 150 daltonian xyloses are trapped, and passes through film less than salinity and the water of 100 Dalton molecular weights, obtains concentration and reach Xylose to 10wt%；This step reaches low-pressure energy-saving and concentrates the purpose of Xylose.Concentration reaches the Xylose of 10% and goes down Procedure, the water passed through is done hydrolysis dosing water, is greatly saved energy consumption, saves water resource；Device therefor is that Weifang is clean The Full-automatic reverse-osmosis material concentration device that star Water Management Equipment Ltd. produces.

S9, middle pressure reverse osmosis membrane concentrate: concentration step S8 obtained reaches the Xylose of 10wt% and is pressurized to 3Mpa, enters Entering middle pressure reverse osmosis membrane, medium pressure reverse osmosis membrane uses polyamide material pollution-resistant membrane, and operating pressure is 3.0-7.0MPa, Computer controls the lower pressure that automatically adjusts and carries out secondary concentration, obtains concentration and reaches the Xylose of 20wt%；In this step, concentration reaches Xylose to 20wt% is delivered to next procedure, and permeate does hydrolysis dosing water.This process expense through water per ton Being about 10 yuan, compared with the expense of equal 70 yuan of triple effect evaporation level per ton, every water saves 60 yuan, and the high-quality reclaimed Pure water can directly as tap water supplement.Device therefor be Weifang Jie Xing Water Management Equipment Ltd. produce complete from Dynamic infiltration material concentration device.

S10, MVR evaporation and concentration: concentration step S9 obtained reaches the Xylose of 20wt% and is heated to 60 DEG C, uses Xylose is evaporated concentrating by MVR vaporizer (i.e. mechanical steam recompression vaporizer), obtains the wood that concentration is 40wt% Sugar liquid；During heating, the heat produced when using the hydrolysis of step S3.The heat produced due to water in advance solution makes Xylose be warmed to 60 DEG C, whole evaporation process does not consume raw steam.The power consumption evaporating water per ton is 20-50KW, effectively reduces evaporation expense. MVR vaporizer is different from common single-action falling liquid film or multiple-effect falling film vaporizer, and MVR is monomer evaporator, collects multiple-effect falling film vaporizer , take stagewise to evaporate according to required product concentration difference, i.e. product can not reach institute for the first time after effect body When needing concentration, product is extracted on effect body by effect external body pipeline after leaving effect body by product by the vacuum pump of effect body bottom Portion is again by effect body, then by this effect body that iterates through to reach desired concn.Imitate the tubule that internal portion is arrangement, pipe Inside is product, and outside is steam, and making product owing to pipe inner area increases in product flow process from top to bottom is film Shape flows, and to increase heating surface area, is imitating internal formation negative pressure by vacuum pump, is reducing the boiling point of water in product, thus reach Concentrating, product evaporating temperature is about 60 DEG C.

S11, chromatographic refining desalination purify: concentration step S10 obtained is the Xylose of 40wt%, and controlling temperature is 50 DEG C, use calcium type chromatographic isolation adsorbent resin to carry out refined desalination and purify, collect extract；Chromatographic isolation adsorbent resin is to xylose Different with the adsorption coefficient of the impurity such as calcium, magnesium, sodium, chlorine, nitrate anion and pigment Deng glucide, cause various material outflow system Time the most different, the component that first flows out is extract (i.e. containing the component that the glucides such as xylose are more), the rear component flowed out Being raffinate (the most impure more component), collect extract and raffinate respectively, extract carries out follow-up xylose to be prepared Processing, after raffinate is concentrated, the side-product as xylose is sold；

S13, concentrate, crystallize, be centrifuged, dry: the Xylose that step S12 is obtained, then use MVR vaporizer and the most single Single-effect evaporator is concentrated into the concentration of 81wt%, the mode of recycling evaporative crystallization to xylose refined liquid, makes xylose massecuite by insatiable hunger Becoming saturated solution with solution and be then converted to supersaturated solution, its xylose crystal grain is constantly grown up and separates out, then by flat from Xylose crystals is separated by scheming with mother solution, respectively obtains xylose crystals and xylose mother liquid, and xylose crystals passes through vibrated fluidized bed will Xylose crystals is dried, and obtains crystalline xylose finished product；Xylose mother liquid is sold as side-product.

In the present embodiment, also include the process step to waste water: use anaerobism, hydrolysis acidification, aerobic, precipitation, light electrolysis, Fenton reagent, flocculation sediment carry out pretreatment, and mud is extruded by pressure filter, is delivered to Organic fertilizer production line；After waste water reaches The inflow requirement of continuous equipment, then after using secondary filter, ultrafiltration, nanofiltration, reverse osmosis advanced process, through water fully recovering to giving birth to Produce line；Condensed water is delivered to the explosion of fodder production line and sprays saline in advance thus realize recycling of waste water.Technology used is the Weihe River The waste water zero-discharge technology that Fang Jie star Water Management Equipment Ltd. provides, Fu Yan mountain, Weifang landfill leachate treatment, Coal gas sewage treatment plant of Shenyang Faku County, the success pilot scale of Changyi Xin Ao Chemical Co., Ltd. or enforcement.

Embodiment 2

A kind of xylose production process, comprises the steps:

S1, pre-treatment: first selecting crude drugs with winnower processes, and then utilizes roller screen to process, finally carries out clean water；Utilize selecting crude drugs with winnower permissible Remove the light impurities such as the Stigma Maydis in corn cob, leaves, plastic bag, remove the dust in corn cob, masonry, Semen Maydis with roller screen The big ratio heavy seeds such as grain, recycling clean water falls the impurity such as dust remaining in corn cob；

Concrete steam explosion step is: utilized at the steam explosion intracavity of steam explosion equipment by the corn cob being sprayed with hydrochloric acid Saturated vapor and air are heated to 120 DEG C, reach pressure 1.5Mpa, pressurize 10 minutes, then when instant decompression is spurted, produce secondary Steam, raw material volume surges, and is acted on by mechanical force, and its solid material is destructurized.Steam explosion of the present invention sets Standby (model is QB1500-3), refers to the steam explosion equipment of commercially available Chinese Academy of Sciences's process engineering institute invention, can be Material is crushed by the moment of 0.00785 second.It is of course also possible to use other steam similar, that required effect can be reached Blasting gear.

S3, low temperature hydrochloric acid hydrolyze: the corn cob (moisture content 30%) through step S2 Steam explosion pretreatment is imported water In solution equipment, adding the hydrochloric acid solution of 0.4wt%, then pass to steam, be warming up to 105 DEG C and stop steam, pressure is 0.15Mpa, It is incubated 2 hours, obtains being mixed with the hydrolysis melt cinder of hydrolyzed solution；Wherein, the hydrochloric acid solution of 0.4wt% can use solid hydrolysis residue Washing liquid configures；Corn cob material dry weight is 1:4 with the weight ratio of the hydrochloric acid solution of 0.4wt%.This step makes in corn cob Hemicellulose and the oligosaccharide degraded are fully converted into xylose molecule.Special hydrolytic equipment used is by the red plastics of Cixi The steel lining plastic reactor that container company limited produces, steel lining plastic reactor temperature, pressure controllable, it is 105 DEG C that temperature controls, pressure Power is 0.15Mpa, and the response time is 2 hours, can be adjusted as required.

S5, decolouring neutralize: xylose hydrolysis fluid step S4 obtained, and are delivered to decolouring with acid-proof pump from hydrolyzed solution storage tank In post, activated carbon or macropore decolorizing resin is utilized to be gone by the impurity such as the pigment in xylose hydrolysis fluid, ash, colloid, visible slag stain Remove so that it is light transmittance reaches 50%, and add appropriate NaOH and be adjusted to save PH to 3.5, obtain transparent Decoloration of Xylose liquid；

S8, low pressure reverse osmosis membrance concentration: Xylose step S7 obtained is pressurized to 2.0Mpa, be 100 through molecular weight Daltonian low-pressure reverse osmosis membrane, described low-pressure reverse osmosis membrane uses polyamide material pollution-resistant membrane, and operating pressure is 1.5- 2.0MPa, molecular weight is that 150 daltonian xyloses are trapped, and passes through film less than salinity and the water of 100 Dalton molecular weights, obtains Concentration reaches the Xylose of 10wt%；This step reaches low-pressure energy-saving and concentrates the purpose of Xylose.Concentration reaches the xylose of 10% Liquid goes next procedure, and the water passed through does hydrolysis dosing water, is greatly saved energy consumption, saves water resource；Device therefor is The Full-automatic reverse-osmosis material concentration device that Weifang Jie Xing Water Management Equipment Ltd. produces.

S9, middle pressure reverse osmosis membrane concentrate: concentration step S8 obtained reaches the Xylose of 10wt% and is pressurized to 7Mpa, enters Entering middle pressure reverse osmosis membrane, medium pressure reverse osmosis membrane uses polyamide material pollution-resistant membrane, and operating pressure is 3.0-7.0MPa, Computer controls the lower pressure that automatically adjusts and carries out secondary concentration, obtains concentration and reaches the Xylose of 20wt%；In this step, concentration reaches Xylose to 20wt% is delivered to next procedure, and permeate does hydrolysis dosing water.This process expense through water per ton Being about 10 yuan, compared with the expense of equal 70 yuan of triple effect evaporation level per ton, every water saves 60 yuan, and the high-quality reclaimed Pure water can directly as tap water supplement.Device therefor be Weifang Jie Xing Water Management Equipment Ltd. produce complete from Dynamic infiltration material concentration device.

S10, MVR evaporation and concentration: concentration step S9 obtained reaches the Xylose of 20wt% and is heated to 60 DEG C, uses Xylose is evaporated concentrating by MVR vaporizer (i.e. mechanical steam recompression vaporizer), obtains the wood that concentration is 50wt% Sugar liquid；During heating, the heat produced when using the hydrolysis of step S3.The heat produced due to water in advance solution makes Xylose be warmed to 60 DEG C, whole evaporation process does not consume raw steam.The power consumption evaporating water per ton is 20-50KW, effectively reduces evaporation expense. MVR vaporizer is different from common single-action falling liquid film or multiple-effect falling film vaporizer, and MVR is monomer evaporator, collects multiple-effect falling film vaporizer , take stagewise to evaporate according to required product concentration difference, i.e. product can not reach institute for the first time after effect body When needing concentration, product is extracted on effect body by effect external body pipeline after leaving effect body by product by the vacuum pump of effect body bottom Portion is again by effect body, then by this effect body that iterates through to reach desired concn.Imitate the tubule that internal portion is arrangement, pipe Inside is product, and outside is steam, and making product owing to pipe inner area increases in product flow process from top to bottom is film Shape flows, and to increase heating surface area, is imitating internal formation negative pressure by vacuum pump, is reducing the boiling point of water in product, thus reach Concentrating, product evaporating temperature is about 60 DEG C.

S11, chromatographic refining desalination purify: concentration step S10 obtained is the Xylose of 50wt%, and controlling temperature is 70 DEG C, use calcium type chromatographic isolation adsorbent resin to carry out refined desalination and purify, collect extract；Chromatographic isolation adsorbent resin is to xylose Different with the adsorption coefficient of the impurity such as calcium, magnesium, sodium, chlorine, nitrate anion and pigment Deng glucide, cause various material outflow system Time the most different, the component that first flows out is extract (i.e. containing the component that the glucides such as xylose are more), the rear component flowed out Being raffinate (the most impure more component), collect extract and raffinate respectively, extract carries out follow-up xylose to be prepared Processing, after raffinate is concentrated, the side-product as xylose is sold；

Embodiment 3

A kind of xylose production process, comprises the steps:

Concrete steam explosion step is: utilized at the steam explosion intracavity of steam explosion equipment by the corn cob being sprayed with hydrochloric acid Saturated vapor and air are heated to 120 DEG C, reach pressure 1.3Mpa, pressurize 9 minutes, then when instant decompression is spurted, produce secondary Steam, raw material volume surges, and is acted on by mechanical force, and its solid material is destructurized.Steam explosion of the present invention sets Standby (model is QB1500-3), refers to the steam explosion equipment of commercially available Chinese Academy of Sciences's process engineering institute invention, can be Material is crushed by the moment of 0.00785 second.It is of course also possible to use other steam similar, that required effect can be reached Blasting gear.

S3, low temperature hydrochloric acid hydrolyze: the corn cob (moisture content 30%) through step S2 Steam explosion pretreatment is imported water In solution equipment, adding the hydrochloric acid solution of 0.3wt%, then pass to steam, be warming up to 102 DEG C and stop steam, pressure is 0.13Mpa, It is incubated 1.5 hours, obtains being mixed with the hydrolysis melt cinder of hydrolyzed solution；Wherein, the hydrochloric acid solution of 0.3wt% can use solid to hydrolyze Wash heat liquid configures；Corn cob material dry weight is 1:3 with the weight ratio of the hydrochloric acid solution of 0.3wt%.This step makes in corn cob Hemicellulose and the oligosaccharide degraded be fully converted into xylose molecule.Special hydrolytic equipment used is moulded by Cixi is red The steel lining plastic reactor that material container company limited produces, steel lining plastic reactor temperature, pressure controllable, it is 102 DEG C that temperature controls, Pressure is 0.13Mpa, and the response time is 1.5 hours, can be adjusted as required.

S5, decolouring neutralize: xylose hydrolysis fluid step S4 obtained, and are delivered to decolouring with acid-proof pump from hydrolyzed solution storage tank In post, activated carbon or macropore decolorizing resin is utilized to be gone by the impurity such as the pigment in xylose hydrolysis fluid, ash, colloid, visible slag stain Remove so that it is light transmittance reaches 35%, and add appropriate NaOH and be adjusted to save PH to 3.0, obtain transparent Decoloration of Xylose liquid；

S8, low pressure reverse osmosis membrance concentration: Xylose step S7 obtained is pressurized to 1.7Mpa, be 100 through molecular weight Daltonian low-pressure reverse osmosis membrane, described low-pressure reverse osmosis membrane uses polyamide material pollution-resistant membrane, and operating pressure is 1.5- 2.0MPa, molecular weight is that 150 daltonian xyloses are trapped, and passes through film less than salinity and the water of 100 Dalton molecular weights, obtains Concentration reaches the Xylose of 10wt%；This step reaches low-pressure energy-saving and concentrates the purpose of Xylose.Concentration reaches the xylose of 10% Liquid goes next procedure, and the water passed through does hydrolysis dosing water, is greatly saved energy consumption, saves water resource；Device therefor is The Full-automatic reverse-osmosis material concentration device that Weifang Jie Xing Water Management Equipment Ltd. produces.

S9, middle pressure reverse osmosis membrane concentrate: concentration step S8 obtained reaches the Xylose of 10wt% and is pressurized to 5Mpa, enters Entering middle pressure reverse osmosis membrane, medium pressure reverse osmosis membrane uses polyamide material pollution-resistant membrane, and operating pressure is 3.0-7.0MPa, Computer controls the lower pressure that automatically adjusts and carries out secondary concentration, obtains concentration and reaches the Xylose of 20wt%；In this step, concentration reaches Xylose to 20wt% is delivered to next procedure, and permeate does hydrolysis dosing water.This process expense through water per ton Being about 10 yuan, compared with the expense of equal 70 yuan of triple effect evaporation level per ton, every water saves 60 yuan, and the high-quality reclaimed Pure water can directly as tap water supplement.Device therefor be Weifang Jie Xing Water Management Equipment Ltd. produce complete from Dynamic infiltration material concentration device.

S10, MVR evaporation and concentration: concentration step S9 obtained reaches the Xylose of 20wt% and is heated to 60 DEG C, uses Xylose is evaporated concentrating by MVR vaporizer (i.e. mechanical steam recompression vaporizer), obtains the wood that concentration is 45wt% Sugar liquid；During heating, the heat produced when using the hydrolysis of step S3.The heat produced due to water in advance solution makes Xylose be warmed to 60 DEG C, whole evaporation process does not consume raw steam.The power consumption evaporating water per ton is 20-50KW, effectively reduces evaporation expense. MVR vaporizer is different from common single-action falling liquid film or multiple-effect falling film vaporizer, and MVR is monomer evaporator, collects multiple-effect falling film vaporizer , take stagewise to evaporate according to required product concentration difference, i.e. product can not reach institute for the first time after effect body When needing concentration, product is extracted on effect body by effect external body pipeline after leaving effect body by product by the vacuum pump of effect body bottom Portion is again by effect body, then by this effect body that iterates through to reach desired concn.Imitate the tubule that internal portion is arrangement, pipe Inside is product, and outside is steam, and making product owing to pipe inner area increases in product flow process from top to bottom is film Shape flows, and to increase heating surface area, is imitating internal formation negative pressure by vacuum pump, is reducing the boiling point of water in product, thus reach Concentrating, product evaporating temperature is about 60 DEG C.

S11, chromatographic refining desalination purify: concentration step S10 obtained is the Xylose of 45wt%, control temperature and are 50-70 DEG C, use calcium type chromatographic isolation adsorbent resin to carry out refined desalination and purify, collect extract；Chromatographic isolation adsorbent resin Different with the adsorption coefficient of the impurity such as calcium, magnesium, sodium, chlorine, nitrate anion and pigment to glucides such as xyloses, cause various material stream The time going out system is the most different, and the component first flowed out, extract (i.e. containing the component that the glucides such as xylose are more), flows out afterwards Component raffinate (the most impure more component), collect extract and raffinate respectively, extract carries out follow-up wood Sugar preparation processes, and after raffinate is concentrated, the side-product as xylose is sold；

Embodiment 4

Pretreatment: take 1 ton of corn cob, utilizes selecting crude drugs with winnower to remove the light impurities in corn cob, removes in corn cob with roller screen Dust, masonry, the big ratio heavy seeds such as niblet, recycling clean water falls in corn cob the impurity such as the dust of remaining.

Steam explosion: the corn cob through pretreatment sprays into the hydrochloric acid of 0.28wt%, imports to have been heated to preset The steam explosion intracavity of temperature, is passed through saturated vapor and air, and controlling temperature is 120 DEG C, and pressure is 1.2Mpa, after pressurize to 9 minute, The valve being connected with receptor, moment pressure release is quickly opened the moment of 0.00785 second.Make hemicellulose in corn cob, wooden Separately, hemicellulose degradation is oligosaccharide (the most oligomeric the eleventh of the twelve Earthly Branches sugar) for element, cellulose；Lignin active group increases and and fiber Element loosens from structure and separates, and makes cellulose crystallity strengthen, creates condition for refined xylose；Green for utilizing hydrolysis residue to manufacture Color glue-free environment friendly artificial board material creates condition.

Low temperature hydrochloric acid hydrolyzes: import in special hydrolysis device by the corn cob (moisture content 30%) through steam explosion, by jade The 1:2 of rice core dry weight adds the hydrochloric acid solution 2 tons of 0.25% with the configuration of hydrolysis residue washing liquid, then passes to steam, heats up Stop steam to 105 DEG C, open compressed air and boost to 0.15Mpa, be incubated 1 hour, make the hemicellulose in corn cob and The oligosaccharide of explanation is fully converted into xylose molecule；

Solid-liquid separation: hydrolysis melt cinder is sent in press type equipment for separating liquid from solid and carries out solid-liquid separation, the xylose after separation Hydrolyzed solution enters hydrolysis flow container, carries out the refinement treatment of next procedure.Hydrolysis residue once purged feeding fermentation tank after separation enters Row solid fermentation, carries out deep activation to lignin, creates conditions for being not added with any adhesive compacting environmental protection artificial board. Hydrolysis residue cleanout fluid reclaims, and after configuration hydrochloric acid solution is hydrolyzed new quick-fried broken corn cob, to reclaim residual sugar, to save water resource；

Decolouring neutralizes: is delivered to fill in decolorizing column by the xylose hydrolysis fluid in hydrolysis flow container with acid-proof pump, utilizes activated carbon By Impurity removals such as the pigment in xylose hydrolysis fluid, ash, colloid, visible slag stains so that it is light transmittance reaches 20%, obtains transparent Decoloration of Xylose liquid；And add appropriate NaOH be adjusted to save PH to 3.5；

Ultra-filtration filters: utilize the semi permeability characteristic of ultrafilter membrane, select the ultrafilter membrane of 20000 Dalton molecular weights, to molecule Amount separates more than 20000 daltonian all impurity and pigment, obtains the Xylose that light transmittance is 80% of clarification, for rear Continuous film processes and creates conditions；

Electrodialysis desalination: utilize the nonconducting characteristic of xylose solution itself, under the effect of DC electric field, N-process produces The zwitterion that raw salt and hydrolytic process produce is removed through anode membrane and cavity block respectively, obtains the water based on xylose and water Solve liquid.The zwitterion that this process will be removed in 80-90% hydrolyzed solution, exchanges refined reduction for follow-up chromatographic refining and ion Burden, decreases the discharge of soda acid；

Low pressure reverse osmosis membrance concentration: through the hydrolyzed solution of electrodialysis process, electrical conductivity is reduced to by 10000us/cm About 1000us/cm.Xylose is pressurized to 1.5-2.0Mpa, is 100 daltonian anti-pollution reverse osmosis membranes through molecular weight, Molecular weight is that 150 daltonian xyloses are trapped, and passes through film less than salinity and the water of 100 Dalton molecular weights, thus reaches low Press the purpose of energy-conservation concentration Xylose.Concentration reaches the Xylose of 10% and goes next procedure, and the water passed through is done hydrolysis dosing and used Water, is greatly saved energy consumption, saves water resource；

Middle pressure reverse osmosis membrane concentrates: the Xylose that concentration reaches 10% is pressurized to 3Mpa, enters anti-pollution reverse osmosis membrane, The most automatically adjusting pressure and carry out secondary concentration, concentration reaches the Xylose of 20% and is delivered to next procedure, passes through Liquid does hydrolysis dosing water.

MVR evaporation and concentration: MVR vaporizer is different from common single-action falling liquid film or multiple-effect falling film vaporizer, MVR is monomer evaporation Device, integrates multiple-effect falling film vaporizer, takes stagewise to evaporate according to required product concentration difference, and i.e. product is at first time warp When can not reach desired concn after crossing effect body, product leave effect body after by effect body bottom vacuum pump by product by effect body Exterior line be extracted into effect body top again by effect body, then by this iterate through effect body to reach desired concn.Effect body The internal tubule for arrangement, pipe is internal is product, and outside is steam, due to pipe inner face in product flow process from top to bottom Amassing increase and making product is membranaceous flowing, to increase heating surface area, is imitating internal formation negative pressure by vacuum pump, is reducing in product The boiling point of water, thus reach to concentrate, product evaporating temperature is about 60 DEG C.Will be through concentrating with the used heat produced in hydrolytic process Xylose be warmed to 60 DEG C, use MVR vaporizer (i.e. mechanical steam recompression vaporizer) be the xylose of 20% to concentration Liquid is evaporated concentrating so that it is dry concentration is 40 50%,.Owing to water in advance solution used heat makes Xylose be warmed to 60 DEG C, Whole evaporation process does not consume raw steam.The power consumption evaporating water per ton is 20-50KW, effectively reduces evaporation expense.

Chromatographic refining desalination purifies: use chromatographic isolation adsorbent resin that xylose MVR evaporation and concentration liquid carries out refined desalination Purify, the chromatographic isolation adsorbent resin absorption system to impurity such as the glucides such as xylose and calcium, magnesium, sodium, chlorine, nitrate anion and pigments Number difference, the time causing various material outflow system is the most different, has after first having, and the component first flowed out (i.e. contains wood extract The component that the glucides such as sugar are more), the rear component flowed out, raffinate (the most impure more component), collects extracting respectively Liquid and raffinate, extract carries out follow-up xylose preparation and processes, and after raffinate is concentrated, the side-product as xylose is sold；

Anion and cation exchange resin refines: by extract by equipped with cloudy (D296), sun (001-7) ion exchange resin The ion exchange column being composed in series, carries out further refinement treatment to Xylose, to remove its anions and canons contained, this The electrical conductivity of process Xylose is less than 5us/cm；

Concentrate, crystallize, be centrifuged, dry: the Xylose concentration exchanged after refining through chromatographic refining and ion decreases, Use MVR vaporizer and continuous single effect evaporator that xylose refined liquid is concentrated into the concentration of 81-84%, recycle evaporative crystallization Mode, make xylose massecuite be become saturated solution from unsaturated solution and be then converted to supersaturated solution, its xylose crystal grain is the longest Big and separate out, then by flat centrifuge, xylose crystals is separated with mother solution, obtain 0.095 ton of xylose crystals and 0.090 ton Concentration is the xylose mother liquid of 60%, and xylose crystals by the moisture removal in xylose crystals, obtains crystallization wood by vibrated fluidized bed Sugar finished product, its moisture content is 0.1% to meet national standard, and xylose mother liquid is sold as side-product.

Waste water processes: use anaerobism, hydrolysis acidification, aerobic, precipitation, light electrolysis, Fenton reagent, flocculation sediment to carry out pre-place Reason, mud is extruded by pressure filter, is delivered to Organic fertilizer production line；Waste water reaches the inflow requirement of follow-up equipment, then uses essence After close filtration, ultrafiltration, nanofiltration, reverse osmosis advanced process, through water fully recovering to production line；Condensed water is delivered to Feed Manufacturing The explosion of line is sprayed saline in advance thus is realized recycling of waste water.

Embodiment 5

Pretreatment: take 0.8 ton of corn cob, utilizes selecting crude drugs with winnower to remove the light impurities in corn cob, removes corn cob with roller screen In dust, masonry, the big ratio heavy seeds such as niblet, recycling clean water falls in corn cob the impurity such as the dust of remaining.

Steam explosion: the corn cob through pretreatment sprays into the hydrochloric acid of 0.18%, imports to have been heated to preset temperature The steam explosion intracavity of degree, is passed through saturated vapor and air, and controlling temperature is 120 DEG C, and pressure is 1.5Mpa, after pressurize to 8 minute, The moment of 0.00785 second quickly opens the valve being connected with receptor, moment pressure release.Make hemicellulose in corn cob, lignin, Separately, hemicellulose degradation is oligosaccharide (the most oligomeric the eleventh of the twelve Earthly Branches sugar) to cellulose；Lignin active group increases and and cellulose Loosen from structure and separate, make cellulose crystallity strengthen, create condition for refined xylose；For utilizing hydrolysis slag to manufacture green Glue-free environment friendly artificial board material creates condition.

Low temperature hydrochloric acid hydrolyzes: import in special hydrolysis device by the corn cob (moisture content 30%) through steam explosion, by jade The 1:6 of rice core dry weight adds the hydrochloric acid solution 4.8 tons of 0.4% with the configuration of hydrolysis residue washing liquid, then passes to steam, heats up Stop steam to 100 DEG C, open compressed air and boost to 0.12Mpa, be incubated 1.3 hours, make the hemicellulose in corn cob and Oligosaccharide through explaining is fully converted into xylose molecule；

Decolouring neutralizes: is delivered to fill in decolorizing column by the xylose hydrolysis fluid in hydrolysis flow container with acid-proof pump, utilizes activated carbon By Impurity removals such as the pigment in xylose hydrolysis fluid, ash, colloid, visible slag stains so that it is light transmittance reaches 20%, obtains transparent Decoloration of Xylose liquid；And add appropriate NaOH be adjusted to save PH to 2.5；

Low pressure reverse osmosis membrance concentration: through the hydrolyzed solution of electrodialysis process, electrical conductivity is reduced to by 10000us/cm About 1000us/cm.Xylose is pressurized to 1.8Mpa, is 100 daltonian anti-pollution reverse osmosis membranes through molecular weight, molecule Amount is that 150 daltonian xyloses are trapped, and passes through film less than salinity and the water of 100 Dalton molecular weights, thus reaches low pressure joint The purpose of Xylose can be concentrated.Concentration reaches the Xylose of 10% and goes next procedure, and the water passed through does hydrolysis dosing water, greatly Save greatly energy consumption, save water resource；

Middle pressure reverse osmosis membrane concentrates: the Xylose that concentration reaches 10% is pressurized to 3.5Mpa, enters anti-pollution reverse-osmosis Film, the most automatically adjusts pressure and carries out secondary concentration, and concentration reaches the Xylose of 20% and is delivered to next procedure, thoroughly Cross liquid and do hydrolysis dosing water.

Concentrate, crystallize, be centrifuged, dry: the Xylose concentration exchanged after refining through chromatographic refining and ion decreases, Use MVR vaporizer and continuous single effect evaporator that xylose refined liquid is concentrated into the concentration of 81-84%, recycling evaporative crystallization Mode, makes xylose massecuite be become saturated solution from unsaturated solution and is then converted to supersaturated solution, and its xylose crystal grain is constantly grown up And separate out, then by flat centrifuge, xylose crystals is separated with mother solution, obtain 0.075 ton of xylose crystals and 0.070 ton dense Degree is the xylose mother liquid of 50%, and xylose crystals by the moisture removal in xylose crystals, obtains crystalline xylose by vibrated fluidized bed Finished product, its moisture content is 0.14% to meet national standard, and xylose mother liquid is sold as side-product.

Embodiment 6

Pretreatment: take 0.9 ton of corn cob, utilizes selecting crude drugs with winnower to remove the light impurities in corn cob, removes corn cob with roller screen In dust, masonry, the big ratio heavy seeds such as niblet, recycling clean water falls in corn cob the impurity such as the dust of remaining.

Steam explosion: the corn cob through pretreatment sprays into the hydrochloric acid of 0.18%, imports to have been heated to preset temperature The steam explosion intracavity of degree, is passed through saturated vapor and air, and controlling temperature is 120 DEG C, and pressure is 1.2Mpa, after pressurize to 9 minute, The moment of 0.00785 second quickly opens the valve being connected with receptor, moment pressure release.Make hemicellulose in corn cob, lignin, Separately, hemicellulose degradation is oligosaccharide (the most oligomeric the eleventh of the twelve Earthly Branches sugar) to cellulose；Lignin active group increases and and cellulose Loosen from structure and separate, make cellulose crystallity strengthen, create condition for refined xylose；For utilizing hydrolysis slag to manufacture green Glue-free environment friendly artificial board material creates condition.

Low temperature hydrochloric acid hydrolyzes: import in special hydrolysis device by the corn cob (moisture content 30%) through steam explosion, by jade The 1:2 of rice core dry weight adds the hydrochloric acid solution 1.8 tons of 0.75% with the configuration of hydrolysis residue washing liquid, then passes to steam, rises Temperature stops steam to 100-105 DEG C, opens compressed air and boosts to 1-1.5Mpa, is incubated 12 hours, makes half fibre in corn cob Dimension element and the oligosaccharide explained are fully converted into xylose molecule；

3, solid-liquid separation: hydrolysis melt cinder is sent in press type equipment for separating liquid from solid and carries out solid-liquid separation, the wood after separation Sugar hydrolyzed solution enters hydrolysis flow container, carries out the refinement treatment of next procedure.Hydrolysis residue once purged feeding fermentation tank after separation Carry out solid fermentation, lignin is carried out deep activation, create bar for being not added with any adhesive compacting environmental protection artificial board Part.Hydrolysis residue cleanout fluid reclaims, and after configuration hydrochloric acid solution is hydrolyzed new quick-fried broken corn cob, to reclaim residual sugar, to save water resource；

Decolouring neutralizes: is delivered to fill in decolorizing column by the xylose hydrolysis fluid in hydrolysis flow container with acid-proof pump, utilizes activated carbon By Impurity removals such as the pigment in xylose hydrolysis fluid, ash, colloid, visible slag stains so that it is light transmittance reaches 20%, obtains transparent Decoloration of Xylose liquid；And add appropriate NaOH be adjusted to save PH to 2.5-3.5；

Middle pressure reverse osmosis membrane concentrates: the Xylose that concentration reaches 10% is pressurized to 3-7Mpa, enters anti-pollution reverse-osmosis Film, the most automatically adjusts pressure and carries out secondary concentration, and concentration reaches the Xylose of 20% and is delivered to next procedure, thoroughly Cross liquid and do hydrolysis dosing water.

MVR evaporation and concentration: MVR vaporizer is different from common single-action falling liquid film or multiple-effect falling film vaporizer, MVR is monomer evaporation Device, integrates multiple-effect falling film vaporizer, takes stagewise to evaporate according to required product concentration difference, and i.e. product is at first time warp When can not reach desired concn after crossing effect body, product leave effect body after by effect body bottom vacuum pump by product by effect body Exterior line be extracted into effect body top again by effect body, then by this iterate through effect body to reach desired concn.

Imitating the tubule that internal portion is arrangement, pipe is internal is product, and outside is steam, at product flow process from top to bottom In owing to pipe inner area increases, to make product be membranaceous flowing, to increase heating surface area, born imitating internal formation by vacuum pump Pressure, reduces the boiling point of water in product, thus reaches to concentrate, and product evaporating temperature is about 60 DEG C.

60 DEG C will be warmed to through the Xylose concentrated with the used heat produced in hydrolytic process, use MVR vaporizer (i.e. machine Tool formula vapor recompression vaporizer) it is evaporated concentrating to the Xylose that concentration is 20% so that it is dry concentration is 40 50%,.Owing to water in advance solution used heat makes Xylose be warmed to 60 DEG C, whole evaporation process does not consume raw steam.Evaporate per ton The power consumption of water is 20-50KW, effectively reduces evaporation expense.

Concentrate, crystallize, be centrifuged, dry: the Xylose concentration exchanged after refining through chromatographic refining and ion decreases, Use MVR vaporizer and continuous single effect evaporator that xylose refined liquid is concentrated into the concentration of 81-84%, recycling evaporative crystallization Mode, makes xylose massecuite be become saturated solution from unsaturated solution and is then converted to supersaturated solution, and its xylose crystal grain is constantly grown up And separate out, then by flat centrifuge, xylose crystals is separated with mother solution, obtain 0.080 ton of xylose crystals and 0.075 ton dense Degree is the xylose mother liquid of 57%, and xylose crystals by the moisture removal in xylose crystals, obtains crystalline xylose by vibrated fluidized bed Finished product, its moisture content is 0.2% to meet national standard, and xylose mother liquid is sold as side-product.

Comparative example

Using traditional production technology, step is as follows:

1) pulverize: proceed to after corn cob removing dust, remove impurity in pulverizer, maize cob meal is broken to 2-3cm, standby；

2) high-temperature water steaming and decocting: the corn cob after pulverizing imports in high-temperature water cooker, by the 1 of corn cob dry weight: 5-10 adds evaporation condensed water, and opens agitating device, controls speed of agitator and is 10-100 rev/min, is warming up to 80-with steam 110 DEG C, insulation send into equipment for separating liquid from solid after 1-3 hour and carry out solid-liquid separation, high temperature steaming liquid after separation enters Sedimentation tank, Its supernatant is for the outer pretreatment of tank of corn cob, to save industry water resource；High temperature steaming slag after separation enters hydrolysis kettle, Be hydrolyzed operation；

3) hydrolysis: pour in hydrolysis kettle by high temperature steaming slag, is added through anti-by the 1:4-12 of high temperature steaming slag dry weight The fresh water that penetration equipment processed, and add concentrated sulphuric acid, making the sulfuric acid concentration of mixed liquor in hydrolysis kettle is 0.8-1.2%, starts Agitating device, controls speed of agitator and is 10-100 rev/min, then pass to steam, is warming up to 100-120 DEG C, is incubated 2-4 hour Rear feeding equipment for separating liquid from solid carries out solid-liquid separation, and the xylose hydrolysis fluid after separation enters hydrolysis flow container, carries out follow-up refining Process；Hydrolysis residue entrance dross coal multifuel combustion biomass boiler after separation carries out burning and prepares steam, for the steaming of present invention process Send out to concentrate and use；

4) decolouring neutralizes: is beaten to decolouring still or decolorizing column by the xylose hydrolysis fluid in hydrolysis flow container with pump, utilizes decolouring Pigment in xylose hydrolysis fluid is removed by the decolorising agent in still or decolorizing column so that it is light transmittance reaches 20-50%；Utilize calcium carbonate PH value is regulated to 3.5；

5) refined: Decoloration of Xylose liquid to be carried out refinement treatment so that it is electrical conductivity is reduced to 50 below μ s/cm；

6) steam raising concentrates: use multi-effect evaporator and single effect evaporator to be evaporated Xylose concentrating, to dry Concentration is 80-85%, obtains xylose massecuite；

8) crystallize, be centrifuged, dry: use the mode of cooling crystallization, carry out cooling knot by the cooling rate of 1 DEG C/h Crystalline substance, makes xylose massecuite be become saturated solution from unsaturated solution and is then converted to supersaturated solution, and its xylose crystal grain is constantly grown up also Separate out, by link-suspended basket centrifuge, xylose crystals is separated with mother solution, respectively obtain xylose crystals and xylose mother liquid, xylose crystals Again by steam drying device by the moisture removal in xylose crystals, obtain crystalline xylose finished product；Xylose mother liquid is as side-product Sell, for preparing the raw material of caramel color product.

Traditional handicraft former material adjuvant, solid waste, waste water, consumption indicators (ton sugar)

As a example by embodiment 3, compared with comparative example, there is following significant progress: embodiment 3 former material adjuvant, solid Useless, waste water, consumption indicators have all had the biggest saving.

Sequence number	Title	Unit	Quantity	Saving rate
					1	Corn cob	Ton	9	10%
2	Steam	Ton	23	64.5%
					3	Electricity	Ton	1100	41.7%
4	Water	Ton	60	90%
					5	Sulphuric acid	Ton	0	100%
6	Activated carbon	Ton	0.045	50%
					7	Calcium carbonate	Ton	0	100%
8	Hydrochloric acid	Ton	0.5	15%
					9	Sodium hydroxide	Ton	0.7	26.3%
10	Ethanol	Ton	0	100%
					11	Solid waste	Ton	Nothing
12	Waste water	Ton	Reuse

Should be appreciated that the purposes of these embodiments is merely to illustrate the present invention and is not intended to limit the protection model of the present invention Enclose.Additionally, it will also be appreciated that after the technology contents having read the present invention, the present invention can be made respectively by those skilled in the art Planting change, amendment and/or modification, all these equivalent form of value falls within the guarantor that the application appended claims is limited equally Within the scope of protecting.

Claims

1. an xylose production process, it is characterised in that: utilize corn cob as raw material, sequentially pass through and include steam explosion, salt Acid hydrolysis, solid-liquid separation, decolouring neutralization, ultra-filtration filters, electrodialysis desalination, low pressure reverse osmosis membrance concentration, middle pressure reverse osmosis membrane are dense Contracting, MVR evaporation and concentration, chromatographic refining desalination purify, ion exchange resin refines, concentrates, crystallizes, is centrifuged, dries in interior step Suddenly, xylose product is finally given.

2. a kind of xylose production process as claimed in claim 1, it is characterised in that: comprise the steps:

S1, pre-treatment: take corn cob as raw material, first selecting crude drugs with winnower process, and then utilize roller screen to process, finally carry out clear water clear Wash；

S2, Steam explosion pretreatment: the corn cob through the pre-treatment of step S1 is sprayed hydrochloric acid, imports the most heated steam explosion chamber In, it is passed through saturated vapor and material is heated by air, under uniform temperature and pressure, after maintaining certain time, moment lets out Pressure；

S3, low temperature hydrochloric acid hydrolyze: import in hydrolysis device by the corn cob through step S2 Steam explosion pretreatment, add The hydrochloric acid solution of 0.2 0.4wt%, then passes to steam, is warming up to 100-105 DEG C and stops steam, and pressure is 0.1-0.15Mpa, It is incubated 12 hours, obtains being mixed with the hydrolysis melt cinder of hydrolyzed solution；

Corn cob material dry weight is 1:(2 4 with the weight ratio of the hydrochloric acid solution of 0.2 0.4wt%)；

S4, solid-liquid separation: step S3 is obtained be mixed with hydrolyzed solution hydrolysis melt cinder send into press type equipment for separating liquid from solid or Carrying out solid-liquid separation, isolated xylose hydrolysis fluid in gasbag-type equipment for separating liquid from solid, xylose hydrolysis fluid enters hydrolyzed solution storage tank, Carry out the refinement treatment of next procedure；The solid hydrolysis residue obtained after separation is carried out, and cleanout fluid reclaims, for configuration step Hydrochloric acid solution in S3；

S5, decolouring neutralize: xylose hydrolysis fluid step S4 obtained, and are delivered to decolorizing column with acid-proof pump from hydrolyzed solution storage tank In, utilize activated carbon or macropore decolorizing resin by Impurity removals such as the pigment in xylose hydrolysis fluid, ash, colloid, visible slag stains, Make its light transmittance reach 20 50%, and add appropriate NaOH and be adjusted to save PH to 2.5-3.5, obtain transparent Decoloration of Xylose Liquid；

S6, ultra-filtration filters: Decoloration of Xylose liquid step S5 obtained, utilize the semi permeability characteristic of ultrafilter membrane, selects the molecular weight to be 20000 daltonian clean star ultrafilter membranes, separate more than 20000 daltonian all impurity and pigment molecular weight, obtain The Xylose of clarification, processes for follow-up film and creates conditions；

S7, electrodialysis desalination: Xylose step S6 obtained, utilize the nonconducting characteristic of Xylose itself, in DC electric field Effect under, salt that N-process produces and the zwitterion that hydrolytic process produces are removed through anode membrane and cavity block respectively, To the Xylose based on xylose and water；

S8, low pressure reverse osmosis membrance concentration: Xylose step S7 obtained is pressurized to 1.5-2.0Mpa, be 100 through molecular weight Daltonian low-pressure reverse osmosis membrane, molecular weight is that 150 daltonian Xyloses are trapped, less than the salt of 100 Dalton molecular weights Divide and water is through film, obtain concentration and reach the Xylose of 10wt%；

S9, middle pressure reverse osmosis membrane concentrate: concentration step S8 obtained reaches the Xylose of 10wt% and is pressurized to 3-7Mpa, enter Middle pressure reverse osmosis membrane, the most automatically adjusts pressure and carries out secondary concentration, obtain concentration and reach the Xylose of 20wt%；

In this step, concentration reaches the Xylose of 20wt% and is delivered to next procedure, and permeate does hydrolysis dosing water；

S10, MVR evaporation and concentration: concentration step S9 obtained reaches the Xylose of 20wt% and is heated to 60 DEG C, uses MVR to steam Send out device to be evaporated Xylose concentrating, obtain the Xylose that concentration is 40 50wt%；

During heating, the heat produced when using the hydrolysis of step S3；

S11, chromatographic refining desalination purify: concentration step S10 obtained is the Xylose of 40 50wt%, control temperature and are 50-70 DEG C, use chromatographic isolation adsorbent resin to carry out refined desalination and purify, collect extract；

S12, ion exchange resin are refined: extract step S11 obtained is by the ion exchange resin equipped with anions and canons The ion exchange column being composed in series, carries out further refinement treatment to extract, to remove its anions and canons contained, To the electrical conductivity Xylose less than 5us/cm；

S13, concentrate, crystallize, be centrifuged, dry: the Xylose that step S12 is obtained, then use MVR vaporizer and continuous single-action to steam Send out device and xylose refined liquid is concentrated into the concentration of 81-84wt%, the mode of recycling evaporative crystallization, make xylose massecuite by unsaturation Solution becomes saturated solution and is then converted to supersaturated solution, and its xylose crystal grain is constantly grown up and separates out, then by flat centrifugal Xylose crystals is separated by machine with mother solution, respectively obtains xylose crystals and xylose mother liquid, and xylose crystals passes through vibrated fluidized bed by wood Sugar crystal is dried, and obtains crystalline xylose finished product；Xylose mother liquid is sold as side-product.

3. a kind of xylose production process as claimed in claim 2, it is characterised in that: also include the process step to waste water: adopt Carrying out pretreatment with anaerobism, hydrolysis acidification, aerobic, precipitation, light electrolysis, Fenton reagent, flocculation sediment, mud passes through pressure filter pressure Go out, be delivered to Organic fertilizer production line；Waste water reaches the inflow requirement of follow-up equipment, then uses secondary filter, ultrafiltration, nanofiltration, anti- After length of penetration processes, through water fully recovering to production line；Condensed water be delivered to the explosion of fodder production line spray in advance saline from And realize recycling of waste water.

4. a kind of xylose production process as claimed in claim 2, it is characterised in that: in step S2, the jade of hydrochloric acid will be sprayed with Meter Xin utilizes saturated vapor and air to be heated to 120 DEG C at the steam explosion intracavity of steam explosion equipment, reaches pressure 1.1-1.5Mpa, Pressurize 8-10 minute, then when instant decompression is spurted, produce indirect steam, raw material volume surges, and is acted on by mechanical force, its solid Material structure is destroyed.

5. a kind of xylose production process as claimed in claim 4, it is characterised in that: described steam explosion equipment refers to commercially available The steam explosion equipment that model is QB1500-3 of Chinese Academy of Sciences process engineering institute invention, can be the moment of 0.00785 second Material is crushed.

6. a kind of xylose production process as claimed in claim 2, it is characterised in that: in step S3, low temperature of the present invention Hydrolytic process, completes in steel lining plastic reactor, its temperature, pressure controllable, and temperature controls as 100-105 DEG C., pressure is 0.1-0.15Mpa, the response time is 1-2 hour.

7. a kind of xylose production process as claimed in claim 2, it is characterised in that: in step S4, use equipment for separating liquid from solid Carrying out solid-liquid separation, described equipment for separating liquid from solid uses the one in Atmosphere Presser or hydraulic squeezing press.

8. a kind of xylose production process as claimed in claim 2, it is characterised in that: in step S7, use electrodialysis plant complete Becoming, described electrodialysis plant uses the one in heterogeneous ion-exchange membrane or homogeneous ion-exchange membrane, described electrodialysis plant DC voltage control is at 80-220V.

9. a kind of xylose production process as claimed in claim 2, it is characterised in that: in step S8, described low-pressure reverse osmosis membrane Using polyamide material pollution-resistant membrane, operating pressure is 1.5-2.0MPa.

10. a kind of xylose production process as claimed in claim 2, it is characterised in that: in step S9, medium pressure reverse osmosis membrane Polyamide material pollution-resistant membrane, operating pressure is 3.0-7.0MPa.