CN107973711A - A kind of method of Simulation moving bed separating glucose acid mother liquid of sodium - Google Patents

A kind of method of Simulation moving bed separating glucose acid mother liquid of sodium Download PDF

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Publication number
CN107973711A
CN107973711A CN201711175286.7A CN201711175286A CN107973711A CN 107973711 A CN107973711 A CN 107973711A CN 201711175286 A CN201711175286 A CN 201711175286A CN 107973711 A CN107973711 A CN 107973711A
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sodium
mother liquid
acid mother
gluconic acid
moving bed
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赵伟
范秀旺
任万松
段莹莹
马春燕
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SHANDONG FUYANG BIOTECHNOLOGY CO Ltd
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SHANDONG FUYANG BIOTECHNOLOGY CO Ltd
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/41—Preparation of salts of carboxylic acids
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/42—Separation; Purification; Stabilisation; Use of additives
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/42—Separation; Purification; Stabilisation; Use of additives
    • C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Saccharide Compounds (AREA)

Abstract

The invention discloses a kind of method of Simulation moving bed separating glucose acid mother liquid of sodium, comprise the following steps：Gluconic acid mother liquid of sodium is diluted with water, and uses activated carbon decolorizing；Gluconic acid mother liquid of sodium after activated carbon decolorizing carries out ion exchange, concentration；Simulation moving bed separating glucose acid mother liquid of sodium, obtains gluconic acid；Gluconic acid is neutralized with sodium hydroxide, obtains sodium gluconate, heating is concentrated to give sodium gluconate solution；The sodium gluconate solution of crystallization, separation and dry gained, obtains sodium gluconate finished product.The method of separating glucose acid mother liquid of sodium of the present invention, the sodium gluconate rate of recovery 91%, and external source chemicals is not added, waste liquid is harmless water body, and equipment is simple, of low cost, remarkable benefit, improves the production level of sodium gluconate, reduces the wasting of resources.

Description

A kind of method of Simulation moving bed separating glucose acid mother liquid of sodium
Technical field
The present invention relates to field of chemical engineering, and in particular to a kind of side of Simulation moving bed separating glucose acid mother liquid of sodium Method.
Background technology
Simulation moving bed is a kind of mass transfer apparatus that liquid lock out operation is carried out using absorption principle.It is continuous with adverse current Mode of operation, by converting the material import and export position of fixed bed adsorption equipment, produces and is continuously moved down equivalent to adsorbent, And the effect that material continuously moves up.Production capacity and separative efficiency the ratio fixed adsorption bed of this equipment are high, and can avoid Channel between moving bed adsorption abrasion, fragment or dust occluding device or pipeline and solid particle seam.
Gluconic acid mother liquid of sodium is remaining waste liquid after extraction sodium gluconate finished product, and specific source is using glucose as original Material, the sodium gluconate liquid produced using fermentation, by filtering, is decolourized, concentrated, crystallization, centrifugation contains gluconic acid The liquid of sodium, that is, gluconic acid mother liquid of sodium.Gluconic acid mother liquid of sodium is after being repeated several times Crystallization Separation, and solid content contains in liquid Measure as 40%-60%, wherein the sodium gluconate containing 30%-40%, 5-15% is polysaccharide, the glucose of 1-5%.But Due to mother liquor large viscosity, impurity is more, and COD contents are high, and that further extracts is difficult.Therefore existing gluconic acid mother liquid of sodium Concrete admixture can only be used as, sells to construction site or concrete admixture manufacturer, in recent years due to local building row Industry is depressed and additive addition requires strictly, can only be closely limited using dosage along with concrete admixture is done, and causes Gluconic acid mother liquid of sodium is unsalable, and directly exhausts and can waste the resources and pollute the environment, so needing a kind of easy place of comparison The method that reason utilizes gluconic acid mother liquid of sodium.
Simulation moving bed is applied to the separation of gluconic acid mother liquid of sodium by the present invention, is a kind of quick, efficient, low consumption point From method.
The content of the invention
Gluconic acid mother liquid of sodium is not dealt with for solution existing process existing in the prior art and causes the wasting of resources, Or simple process, it is separated go out sodium gluconate purity is not high and technical problem that the rate of recovery is low, the present invention provides one kind The method of Simulation moving bed separating glucose acid mother liquid of sodium.
To achieve these goals, the present invention adopts the following technical scheme that：
A kind of method of Simulation moving bed separating glucose acid mother liquid of sodium, comprises the following steps：
1) gluconic acid mother liquid of sodium is diluted with water, and uses activated carbon decolorizing；
2) the gluconic acid mother liquid of sodium after activated carbon decolorizing carries out ion exchange, concentration；
3) Simulation moving bed separating glucose acid mother liquid of sodium, obtains gluconic acid；
4) gluconic acid is neutralized with sodium hydroxide solution, obtains sodium gluconate, heating is concentrated to give glucose Acid sodium solution；
5) sodium gluconate solution is crystallized, separated and is dried the sodium gluconate solution of gained, obtains gluconic acid Sodium finished product.
Beneficial effects of the present invention are：The sodium gluconate rate of recovery of the present invention is high, separated rear mixed liquor sodium gluconate Content is less than 0.3%, and sodium gluconate purity is higher than 98% after separation, does not add external source chemicals, and waste liquid is harmless water body, Equipment is simple, of low cost, improves the production level of sodium gluconate, reduces the wasting of resources.
150,000 tons of Fu Yang companies sodium gluconate annual output, meter can discharge 100 tons of mother liquors daily, daily using this technique Recyclable sodium gluconate：100 × (30%-40%) × 91%=(27.3-36.4) ton, sodium gluconate Mother liquid by 35000 tons/year are reduced close to zero.
Further, the concrete operations that gluconic acid mother liquid of sodium described in step 1) is diluted with water are：It is female to sodium gluconate The deionized water of 1 times of volume is added in liquid, obtains the fluid foods of 2 times of original volume.
It is above-mentioned further to have the beneficial effect that：Gluconic acid mother liquid of sodium is diluted, easy to decolorization and purification.
Further, the concrete operations of activated carbon decolorizing described in step 1) are：Diluted gluconic acid mother liquid of sodium will be passed through 75-80 DEG C is warming up to, adds the activated carbon of 0.1-0.3% (w/v), stirs 15-30 minutes and decolourizes.
It is above-mentioned further to have the beneficial effect that：Gluconic acid mother liquid of sodium is purified, is effectively adsorbed in gluconic acid mother liquid of sodium Impurity
Further, the concrete operations of ion exchange described in step 2) are：It is female that sodium gluconate is removed with resin cation Na in liquid+、K+And Mg2+。
It is above-mentioned further to have the beneficial effect that：The gluconic acid mother liquid of sodium after decoloration is carried again using resin cation It is pure, fully remove the Na in gluconic acid mother liquid of sodium+、K+And Mg2+。
Further, the separated condition of Simulation moving bed described in step 3) is：65 DEG C, pressure 0.25Mpa of bath temperature, into After sample, 1h starts to collect sample, collects 1h.
It is above-mentioned further to have the beneficial effect that：Using Simulation moving bed, the Portugal in efficient separating glucose acid mother liquid of sodium Grape saccharic acid, separated rear mixed liquor gluconic acid sodium content are less than 0.3%, and separating effect is notable, and separation equipment is simple, and cost is low It is honest and clean.
Further, after the step 3) is additionally included in the isolated gluconic acid of the Simulation moving bed, waste liquid is shifted Marsh gas power generation is carried out to sewage plant.
It is above-mentioned further to have the beneficial effect that：Waste liquid is harmless water body, and waste liquid is made full use of, reduces the wasting of resources.
Further, the mass concentration of sodium hydroxide solution described in step 4) is 30%, the specific behaviour of the heating concentration As：Sodium gluconate solution is heated to 105-115 DEG C, and is concentrated into gluconic acid sodium content up to more than 70%.
It is above-mentioned further to have the beneficial effect that：Gluconic acid is set fully to react for sodium gluconate, the gluconic acid of gained Sodium purity is higher than 98%.
Further, crystallized described in step 5), separation and the concrete operations of dried grape saccharic acid sodium solution are：By the Portugal Grape saccharic acid sodium solution is cooled to 75 DEG C and starts to crystallize, and crystal is separated with liquid, dry.
It is above-mentioned further to have the beneficial effect that：Make sodium gluconate sufficient crystallising.
Brief description of the drawings
Fig. 1 is the method flow schematic diagram of Simulation moving bed separating glucose acid mother liquid of sodium of the present invention.
Embodiment
Below in conjunction with the attached drawing in the embodiment of the present invention, the technical solution in the embodiment of the present invention is carried out clear, complete Site preparation describes, it is clear that described embodiment is only part of the embodiment of the present invention, instead of all the embodiments.Based on this Embodiment in invention, the every other reality that those of ordinary skill in the art are obtained without making creative work Example is applied, belongs to the scope of protection of the invention.
Sodium gluconate is produced with the prior art, and obtains gluconic acid mother liquid of sodium.
Cornstarch is dissolved into starch milk (18-20 ° of B é of Baume degrees), add 0.5 ‰ a- amylase stir evenly after With steam mixing jetting, 108 DEG C -110 DEG C of temperature, steam pressure 0.6MPa, makes starch milk liquefy, and is cooled to 60 DEG C, PH is adjusted to 4.2-4.4 adds 0.9 ‰ carbohydrase, and stirring saccharification 30 obtains glucose when small.Add 30% glucose and battalion in fermentation tank Support salt, sterilizing cooling, the aspergillus niger seed liquor that access volume fraction is 15%, 36 DEG C of fermentation jar temperature, tank pressure 0.08mpa, stream Be hydrogenated with sodium oxide molybdena, PH is maintained 5.5-6.0, stir and ventilation condition under ferment that about 25-30 is small when.Black-koji mould is by grape Glycosyloxy is melted into gluconic acid, by being constantly pumped into sodium hydroxide solution, the neutralized reaction of gluconic acid is changed into gluconic acid Sodium, the fermentation ends when residual sugar is down to ＜ 10g/L.Filter aid plate-frame filtering is added in zymotic fluid and removes mycelium, in heating 70 DEG C, PH7.0 is adjusted, adds activated carbon decolorizing, filtering is completed in decoloration, and 105-115 DEG C of filtrate sodium gluconate is concentrated into more than 70% Content, crystallisation by cooling.Seperator separates crystal with liquid, and crystal obtains sodium gluconate finished product through fluidized bed drying, remaining Liquid be gluconic acid mother liquid of sodium, gluconic acid mother liquid of sodium is sometimes for Crystallization Separation is repeated several times, fully to extract Portugal Grape sodium saccharate.
The gluconic acid mother liquid of sodium that above-mentioned steps are extracted after measured, solid content 49%, gluconic acid sodium content 31%, (molecular formula C6H11O7Na, molecular weight 218) total sugar content 6.6%, wherein glucose content 1.3%, (molecular formula C6H12O6, molecular weight 180) disaccharides, three sugared contents (in terms of disaccharides) 4.9%, (molecular formula C12H22O11·H2O, molecular weight 360) four Sugar, five sugared contents 0.29%, molecular weight are more than 540, and protein content 0.1%, molecular weight is more than 900, content of ashes 12%.
Embodiment 1
1) deionized water of 1 times of volume is added into gluconic acid mother liquid of sodium, the sodium gluconate for obtaining 2 times of original volume is female Liquid dilution, will be warming up to 75 DEG C by diluted gluconic acid mother liquid of sodium, add the activated carbon of 0.1% (w/v), stir 15 points Clock decolourizes；
2) Na in the gluconic acid mother liquid of sodium after activated carbon decolorizing is removed with resin cation+、K+And Mg2+, concentration；
3) Simulation moving bed separating glucose acid mother liquid of sodium, sample introduction under conditions of 65 DEG C of bath temperature, pressure 0.25Mpa Afterwards, 1h starts to collect sample, collects 1h, obtains gluconic acid, and waste liquid is transferred to sewage plant carries out marsh gas power generation；
4) gluconic acid is neutralized with the sodium hydroxide solution that mass concentration is 30%, it is molten obtains sodium gluconate Liquid, heating sodium gluconate solution are concentrated into gluconic acid sodium content up to more than 70% to 105 DEG C；
5) above-mentioned sodium gluconate solution is cooled to 75 DEG C to start to crystallize, and crystal is separated with liquid, it is dry, obtain Sodium gluconate finished product.
Embodiment 2
1) deionized water of 1 times of volume is added into gluconic acid mother liquid of sodium, the sodium gluconate for obtaining 2 times of original volume is female Liquid dilution, will be warming up to 80 DEG C by diluted gluconic acid mother liquid of sodium, add the activated carbon of 0.3% (w/v), stir 30 points Clock decolourizes；
2) Na in the gluconic acid mother liquid of sodium after activated carbon decolorizing is removed with resin cation+、K+And Mg2+, concentration；
3) Simulation moving bed separating glucose acid mother liquid of sodium, sample introduction under conditions of 65 DEG C of bath temperature, pressure 0.25Mpa Afterwards, 1h starts to collect sample, collects 1h, obtains gluconic acid, and waste liquid is transferred to sewage plant carries out marsh gas power generation；
4) gluconic acid is neutralized with the sodium hydroxide solution that mass concentration is 30%, it is molten obtains sodium gluconate Liquid, heating sodium gluconate solution are concentrated into gluconic acid sodium content up to more than 70% to 115 DEG C；
5) above-mentioned sodium gluconate solution is cooled to 75 DEG C to start to crystallize, and crystal is separated with liquid, it is dry, obtain Sodium gluconate finished product.
Embodiment 3
1) deionized water of 1 times of volume is added into gluconic acid mother liquid of sodium, the sodium gluconate for obtaining 2 times of original volume is female Liquid dilution, will be warming up to 76 DEG C by diluted gluconic acid mother liquid of sodium, add the activated carbon of 0.2% (w/v), stir 17 points Clock decolourizes；
2) Na in the gluconic acid mother liquid of sodium after activated carbon decolorizing is removed with resin cation+、K+And Mg2+, concentration；
3) Simulation moving bed separating glucose acid mother liquid of sodium, sample introduction under conditions of 65 DEG C of bath temperature, pressure 0.25Mpa Afterwards, 1h starts to collect sample, collects 1h, obtains gluconic acid, and waste liquid is transferred to sewage plant carries out marsh gas power generation；
4) gluconic acid is neutralized with the sodium hydroxide solution that mass concentration is 30%, it is molten obtains sodium gluconate Liquid, heating sodium gluconate solution are concentrated into gluconic acid sodium content up to more than 70% to 108 DEG C；
5) above-mentioned sodium gluconate solution is cooled to 75 DEG C to start to crystallize, and crystal is separated with liquid, it is dry, obtain Sodium gluconate finished product.
Embodiment 4
1) deionized water of 1 times of volume is added into gluconic acid mother liquid of sodium, the sodium gluconate for obtaining 2 times of original volume is female Liquid dilution, will be warming up to 77 DEG C by diluted gluconic acid mother liquid of sodium, add the activated carbon of 0.3% (w/v), stir 16 points Clock decolourizes；
2) Na in the gluconic acid mother liquid of sodium after activated carbon decolorizing is removed with resin cation+、K+And Mg2+, concentration；
3) Simulation moving bed separating glucose acid mother liquid of sodium, sample introduction under conditions of 65 DEG C of bath temperature, pressure 0.25Mpa Afterwards, 1h starts to collect sample, collects 1h, obtains gluconic acid, and waste liquid is transferred to sewage plant carries out marsh gas power generation；
4) gluconic acid is neutralized with the sodium hydroxide solution that mass concentration is 30%, it is molten obtains sodium gluconate Liquid, heating sodium gluconate solution are concentrated into gluconic acid sodium content up to more than 70% to 106 DEG C；
5) above-mentioned sodium gluconate solution is cooled to 75 DEG C to start to crystallize, and crystal is separated with liquid, it is dry, obtain Sodium gluconate finished product.
Embodiment 5
1) deionized water of 1 times of volume is added into gluconic acid mother liquid of sodium, the sodium gluconate for obtaining 2 times of original volume is female Liquid dilution, will be warming up to 78 DEG C by diluted gluconic acid mother liquid of sodium, add the activated carbon of 0.2% (w/v), stir 19 points Clock decolourizes；
2) Na in the gluconic acid mother liquid of sodium after activated carbon decolorizing is removed with resin cation+、K+And Mg2+, concentration；
3) Simulation moving bed separating glucose acid mother liquid of sodium, sample introduction under conditions of 65 DEG C of bath temperature, pressure 0.25Mpa Afterwards, 1h starts to collect sample, collects 1h, obtains gluconic acid, and waste liquid is transferred to sewage plant carries out marsh gas power generation；
4) gluconic acid is neutralized with the sodium hydroxide solution that mass concentration is 30%, it is molten obtains sodium gluconate Liquid, heating sodium gluconate solution are concentrated into gluconic acid sodium content up to more than 70% to 117 DEG C；
5) above-mentioned sodium gluconate solution is cooled to 75 DEG C to start to crystallize, and crystal is separated with liquid, it is dry, obtain Sodium gluconate finished product.
Comparative example 1
Take gluconic acid mother liquid of sodium to add 2 times of water dilutions, be warming up to 60 DEG C, the activated carbon for adding 0.2% (w/v) stirs 18 points Clock decolourizes, and is pumped into accurate filter filtering, removes the impurity such as depigmentation, ash content, soluble protein, the clear liquid filtered out is through plate-type heat-exchange Device is cooled to 45 DEG C, is pumped into the nanofiltration device filtering and concentrating of molecular cut off 300Da, removes concentrated phase material, and nanofiltration dislysate enters anti- Osmosis membrane filter filtering and concentrating, obtains concentrated phase material and send two effect decompression evaporator condensing crystallizings, through separating, being dried to obtain technical grade Product.
Performance detection
The gluconic acid of embodiment 1-5 and comparative example 1 by recycling add 30% sodium hydroxide solution to neutralize, by dense Contracting Crystallization Separation is as follows by liquid chromatography analysis, purity：
The sodium gluconate purity analysis result that 1 embodiment 1-5 of table and comparative example 1 recycle
Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Embodiment 5 Comparative example 1
Purity 97.9% 98.3% 98.1% 98.1% 98.0% 97.6%
As shown in Table 1, the separated sodium gluconate purity of the separation method of 1-5 of the embodiment of the present invention is higher than 98%.
Liquid chromatography analysis are made to mixed liquor after separation, analysis result is as follows：
The composition analysis result of mixed liquor after 2 embodiment 1-5 of table and comparative example 1 separate
As shown in Table 2, mixed liquor gluconic acid sodium content is less than after the separation method of 1-5 of the embodiment of the present invention is separated 0.3%, the sodium gluconate rate of recovery is up to 91%.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all the present invention spirit and Within principle, any modification, equivalent replacement, improvement and so on, should all be included in the protection scope of the present invention.

Claims (8)

  1. A kind of 1. method of Simulation moving bed separating glucose acid mother liquid of sodium, it is characterised in that comprise the following steps：
    1) gluconic acid mother liquid of sodium is diluted with water, and uses activated carbon decolorizing；
    2) the gluconic acid mother liquid of sodium after activated carbon decolorizing carries out ion exchange, concentration；
    3) Simulation moving bed separating glucose acid mother liquid of sodium, obtains gluconic acid；
    4) gluconic acid that step 3) obtains is neutralized with sodium hydroxide solution, obtains sodium gluconate, heating is concentrated to give To sodium gluconate solution；
    5) sodium gluconate solution that step 4) obtains is crystallized, separated and dried, and obtains sodium gluconate finished product.
  2. A kind of 2. method of Simulation moving bed separating glucose acid mother liquid of sodium according to claim 1, it is characterised in that step It is rapid 1) described in the concrete operations that are diluted with water of gluconic acid mother liquid of sodium be：1 times of volume of addition into gluconic acid mother liquid of sodium Deionized water, obtains the fluid foods of 2 times of original volume.
  3. A kind of 3. method of Simulation moving bed separating glucose acid mother liquid of sodium according to claim 1, it is characterised in that step It is rapid 1) described in the concrete operations of activated carbon decolorizing be：75-80 DEG C will be warming up to by diluted gluconic acid mother liquid of sodium, will be added The activated carbon of 0.1-0.3% (w/v), stirs 15-30 minutes and decolourizes.
  4. A kind of 4. method of Simulation moving bed separating glucose acid mother liquid of sodium according to claim 1, it is characterised in that step It is rapid 2) described in the concrete operations of ion exchange be：The Na in gluconic acid mother liquid of sodium is removed with resin cation+、K+And Mg2+。
  5. A kind of 5. method of Simulation moving bed separating glucose acid mother liquid of sodium according to claim 1, it is characterised in that step It is rapid 3) described in the separated condition of Simulation moving bed be：65 DEG C, pressure 0.25Mpa of bath temperature, after sample introduction, 1h starts to collect sample Product, collect 1h.
  6. A kind of 6. method of Simulation moving bed separating glucose acid mother liquid of sodium according to claim 1, it is characterised in that institute State after step 3) is additionally included in the isolated gluconic acid of the Simulation moving bed, waste liquid is transferred to sewage plant and carries out biogas hair Electricity.
  7. 7. a kind of method of Simulation moving bed separating glucose acid mother liquid of sodium according to any one of claims 1 to 6, it is special Sign is that the mass concentration of sodium hydroxide solution described in step 4) is 30%, and the concrete operations of the heating concentration are：Heating Sodium gluconate solution is concentrated into gluconic acid sodium content up to more than 70% to 105-115 DEG C.
  8. 8. a kind of method of Simulation moving bed separating glucose acid mother liquid of sodium according to any one of claims 1 to 6, it is special Sign is, is crystallized described in step 5), separation and the concrete operations of dried grape saccharic acid sodium solution are：By the sodium gluconate Solution is cooled to 75 DEG C and starts to crystallize, and crystal is separated with liquid, dry.
CN201711175286.7A 2017-11-22 2017-11-22 A kind of method of Simulation moving bed separating glucose acid mother liquid of sodium Pending CN107973711A (en)

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CN111559765A (en) * 2020-03-31 2020-08-21 东莞市逸轩环保科技有限公司 Comprehensive resource utilization process for liquid-throwing waste liquid

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Publication number Priority date Publication date Assignee Title
CN109369731A (en) * 2018-12-14 2019-02-22 广西福仪生物技术有限公司 A kind of method of glucose during removing xylose production
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CN111559765A (en) * 2020-03-31 2020-08-21 东莞市逸轩环保科技有限公司 Comprehensive resource utilization process for liquid-throwing waste liquid

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