CN117551149A - Method for producing D-ribose and recycling acid and alkali by adenine mother liquor - Google Patents
Method for producing D-ribose and recycling acid and alkali by adenine mother liquor Download PDFInfo
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- CN117551149A CN117551149A CN202311398628.7A CN202311398628A CN117551149A CN 117551149 A CN117551149 A CN 117551149A CN 202311398628 A CN202311398628 A CN 202311398628A CN 117551149 A CN117551149 A CN 117551149A
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- Prior art keywords
- adenine
- ribose
- acid
- alkali
- mother liquor
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- PYMYPHUHKUWMLA-LMVFSUKVSA-N aldehydo-D-ribose Chemical compound OC[C@@H](O)[C@@H](O)[C@@H](O)C=O PYMYPHUHKUWMLA-LMVFSUKVSA-N 0.000 title claims abstract description 127
- GFFGJBXGBJISGV-UHFFFAOYSA-N Adenine Chemical compound NC1=NC=NC2=C1N=CN2 GFFGJBXGBJISGV-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 229930024421 Adenine Natural products 0.000 title claims abstract description 66
- 229960000643 adenine Drugs 0.000 title claims abstract description 65
- PYMYPHUHKUWMLA-UHFFFAOYSA-N arabinose Natural products OCC(O)C(O)C(O)C=O PYMYPHUHKUWMLA-UHFFFAOYSA-N 0.000 title claims abstract description 64
- SRBFZHDQGSBBOR-UHFFFAOYSA-N beta-D-Pyranose-Lyxose Natural products OC1COC(O)C(O)C1O SRBFZHDQGSBBOR-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 239000012452 mother liquor Substances 0.000 title claims abstract description 55
- 239000003513 alkali Substances 0.000 title claims abstract description 52
- 239000002253 acid Substances 0.000 title claims abstract description 49
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 32
- 238000004064 recycling Methods 0.000 title claims abstract description 19
- 239000007788 liquid Substances 0.000 claims abstract description 72
- 239000012528 membrane Substances 0.000 claims abstract description 46
- 150000003839 salts Chemical class 0.000 claims abstract description 41
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 37
- 238000000034 method Methods 0.000 claims abstract description 28
- 239000000706 filtrate Substances 0.000 claims abstract description 27
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000001914 filtration Methods 0.000 claims abstract description 18
- 238000000909 electrodialysis Methods 0.000 claims abstract description 17
- 229920002401 polyacrylamide Polymers 0.000 claims abstract description 14
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 13
- 229920001429 chelating resin Polymers 0.000 claims abstract description 11
- 238000001816 cooling Methods 0.000 claims abstract description 10
- 239000013078 crystal Substances 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 79
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 68
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 57
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 28
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 14
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 11
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 claims description 11
- 239000011575 calcium Substances 0.000 claims description 11
- 229910001424 calcium ion Inorganic materials 0.000 claims description 11
- 238000004090 dissolution Methods 0.000 claims description 11
- 229910001425 magnesium ion Inorganic materials 0.000 claims description 11
- 239000012267 brine Substances 0.000 claims description 10
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims description 10
- 238000002425 crystallisation Methods 0.000 claims description 7
- 230000008025 crystallization Effects 0.000 claims description 7
- 238000006386 neutralization reaction Methods 0.000 claims description 7
- JZTPOMIFAFKKSK-UHFFFAOYSA-N O-phosphonohydroxylamine Chemical compound NOP(O)(O)=O JZTPOMIFAFKKSK-UHFFFAOYSA-N 0.000 claims description 6
- KXDHJXZQYSOELW-UHFFFAOYSA-N Carbamic acid Chemical group NC(O)=O KXDHJXZQYSOELW-UHFFFAOYSA-N 0.000 claims description 5
- 239000010413 mother solution Substances 0.000 claims description 5
- 230000001105 regulatory effect Effects 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- 230000018044 dehydration Effects 0.000 claims description 2
- 238000006297 dehydration reaction Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 239000002585 base Substances 0.000 abstract description 5
- 239000002699 waste material Substances 0.000 abstract description 3
- 238000000855 fermentation Methods 0.000 abstract description 2
- 230000004151 fermentation Effects 0.000 abstract description 2
- 230000000813 microbial effect Effects 0.000 abstract description 2
- OIRDTQYFTABQOQ-KQYNXXCUSA-N adenosine group Chemical group [C@@H]1([C@H](O)[C@H](O)[C@@H](CO)O1)N1C=NC=2C(N)=NC=NC12 OIRDTQYFTABQOQ-KQYNXXCUSA-N 0.000 description 21
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 12
- 229920005989 resin Polymers 0.000 description 11
- 239000011347 resin Substances 0.000 description 11
- KDCGOANMDULRCW-UHFFFAOYSA-N 7H-purine Chemical compound N1=CNC2=NC=NC2=C1 KDCGOANMDULRCW-UHFFFAOYSA-N 0.000 description 10
- 239000002126 C01EB10 - Adenosine Substances 0.000 description 10
- 229960005305 adenosine Drugs 0.000 description 10
- 238000002360 preparation method Methods 0.000 description 10
- 229910017053 inorganic salt Inorganic materials 0.000 description 8
- 239000013522 chelant Substances 0.000 description 6
- 239000011780 sodium chloride Substances 0.000 description 6
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 5
- 239000011521 glass Substances 0.000 description 5
- 238000006460 hydrolysis reaction Methods 0.000 description 5
- 102000004169 proteins and genes Human genes 0.000 description 5
- 108090000623 proteins and genes Proteins 0.000 description 5
- 229910052938 sodium sulfate Inorganic materials 0.000 description 5
- 235000011152 sodium sulphate Nutrition 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 230000007062 hydrolysis Effects 0.000 description 4
- 239000000049 pigment Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000011033 desalting Methods 0.000 description 3
- 239000000839 emulsion Substances 0.000 description 3
- 150000007522 mineralic acids Chemical class 0.000 description 3
- 230000002194 synthesizing effect Effects 0.000 description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 239000012065 filter cake Substances 0.000 description 2
- 230000003301 hydrolyzing effect Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 125000003603 D-ribosyl group Chemical group C1([C@H](O)[C@H](O)[C@H](O1)CO)* 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 238000005349 anion exchange Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000005341 cation exchange Methods 0.000 description 1
- -1 cation ion Chemical class 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010612 desalination reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H3/00—Compounds containing only hydrogen atoms and saccharide radicals having only carbon, hydrogen, and oxygen atoms
- C07H3/02—Monosaccharides
Abstract
The invention belongs to the technical field of microbial fermentation, and particularly relates to a method for producing D-ribose and recycling acid and alkali from adenine mother liquor. The method comprises the following steps: A. adding polyacrylamide solution into adenine mother liquor for pretreatment, adding active carbon to decolorize the adenine mother liquor, and filtering to obtain clear filtrate; B. passing the filtrate from the step A through a chelating resin column to obtain a clarified collecting liquid; C. b, treating the collecting liquid in the step B by using a bipolar membrane to obtain an acid liquid, an alkali liquid and a dilute salt collecting liquid; D. c, treating the dilute salt collecting liquid obtained in the step C by electrodialysis to obtain desalted liquid and concentrated salt water, wherein the desalted liquid is D-ribose solution; E. concentrating, cooling and crystallizing, separating and drying the D-ribose solution in the step D in a concentration furnace to obtain D-ribose crystals. The invention obtains acid-base and D-ribose after the adenine mother liquor is treated, and utilizes the production waste as a resource, thereby being environment-friendly and increasing the economic benefit of enterprises.
Description
Technical Field
The invention belongs to the technical field of microbial fermentation, and particularly relates to a method for producing D-ribose and recycling acid and alkali from adenine mother liquor.
Background
Adenine (Adenine), also known as 6-aminopurine, is one of the four nucleobases that make up DNA and RNA molecules. At present, the main industrial production method of adenine is adenosine hydrolysis method for synthesizing adenine. The Chinese patent application with the application number of 202010325202.9 discloses a method for synthesizing adenine by using an adenosine hydrolysis method, wherein the method comprises the steps of taking adenosine as a raw material, taking inorganic acid (hydrochloric acid and sulfuric acid) as a hydrolysis medium, reacting and separating to obtain the adenine. A large amount of inorganic acid (hydrochloric acid and sulfuric acid) is added in the reaction process, the reaction is neutralized by sodium carbonate or sodium hydroxide, and after adenine is obtained by separation, the residual adenine mother liquor is not disclosed how to treat. Because adenine mother liquor contains a large amount of inorganic salts and D-ribose, the components are complex, the recycling is difficult, the adenine mother liquor is mainly discharged into an environment-friendly workshop for biochemical treatment, and the salt content is high, so that the biochemical treatment efficiency is affected.
Disclosure of Invention
Aiming at the technical defects, the invention solves the problem that the mother solution for synthesizing adenine by the existing adenosine hydrolysis method is difficult to recycle, and simultaneously provides a method for producing D-ribose and recycling acid and alkali by using the adenine mother solution.
In order to solve the technical problems, the technical scheme provided by the invention is as follows: a method for producing D-ribose and recycling acid and alkali by adenine mother liquor comprises the following steps:
A. adding polyacrylamide solution into adenine mother liquor for pretreatment, regulating pH to 6.0-7.0, regulating temperature to 60-70 ℃, adding active carbon to decolorize the adenine mother liquor, stirring for 25-35min, and filtering to obtain clear filtrate; the adenine mother liquor contains macromolecular proteins and residual adenine and adenosine, and the macromolecular proteins and residual adenine and adenosine form emulsion, when the emulsion is directly filtered, the impurities directly penetrate filter cloth, the effect of intercepting the impurities cannot be achieved, after the polyacrylamide solution is added, the polyacrylamide, macromolecular proteins, pigments, residual adenine and adenosine and other suspended matters form a net structure due to the neutralization electrostatic charge and bridging effect, the net structure is captured and organized into larger floccules, the emulsion is aggregated and flocculated, subsequent filtration is facilitated, then activated carbon is added, pigments formed by hydrolysis reaction are easily adsorbed by the activated carbon under the condition of weak acidity pH6.0-7.0, the viscosity of sugar-containing solution is reduced, the molecular movement speed is accelerated, the decoloring efficiency is improved, and diatomite can be added for assisting filtration, so that the floccules form compact filter cakes, and the filtration speed is improved. The step can remove macromolecular proteins and pigments, and remove residual adenine and adenosine, thereby achieving the effect of purifying the filtrate.
B. And C, allowing the filtrate obtained in the step A to flow through a chelating resin column, and adsorbing and separating calcium and magnesium ions in the filtrate to obtain a clear collecting liquid.
C. B, treating the collecting liquid in the step B by using a bipolar membrane to obtain an acid liquid, an alkali liquid and a dilute salt collecting liquid; the conductivity of the dilute salt collecting solution is reduced to 3-3.5mS/cm, and when the conductivity tends to be stable, the bipolar membrane is stopped, the acid liquor returns to the preparation tank to serve as acid and water for adenine mother liquor production, the alkali liquor returns to the preparation tank to serve as water for tablet alkali dissolution, and the prepared alkali liquor serves as neutralization in adenine mother liquor production; the bipolar membrane equipment is provided with three containers, which are generally called a salt chamber, an acid chamber and an alkali chamber respectively, the salt content of the feed liquid to be treated is high, the feed liquid to be treated is put into the salt chamber, after the machine is started, acid liquor is formed in the acid chamber after the bipolar membrane treatment, alkali liquor is formed in the alkali chamber, and the concentrated brine of the original salt chamber is changed into light brine.
D. And C, treating the dilute salt collecting liquid in the step, namely, carrying out electrodialysis, stopping electrodialysis when the conductivity of the dilute salt collecting liquid reaches 50-100 mu S/cm, and obtaining desalted liquid and strong brine, wherein the desalted liquid is D-ribose solution, and the strong brine is returned to the step C, namely, is mixed with the collecting liquid in the step B, and is treated by a bipolar membrane.
E. And D-ribose solution in the step D is concentrated and dehydrated by a concentration furnace, when no obvious water flows out, ethanol with volume of one time is added, the concentration and dehydration are continued, the recovered ethanol containing water is collected, the dehydrated concentrated solution is obtained, and then ethanol is added for dissolution, activated carbon is added for decoloration, filtration, cooling crystallization, separation and drying are carried out, so that D-ribose crystals are obtained.
Further: in the method for producing D-ribose and recycling acid and alkali by using the adenine mother liquor, the addition amount of the polyacrylamide solution in the step A is 0.5-1.0% of the volume percentage of the adenine mother liquor. The weight percentage concentration of the polyacrylamide solution is 0.2%.
The addition amount of the activated carbon in the step A is 0.50-0.65% of the volume percentage of the adenine mother solution.
The chelating resin in the step B is amino carboxylic acid chelating resin or amino phosphoric acid chelating resin. Aiming at the difficult problem of removing calcium and magnesium ions from the filtrate containing D-ribose and inorganic salt, the invention removes the calcium and magnesium ions by utilizing the principle that the calcium and magnesium ions can be combined with specific groups. The traditional chelate resin is usually used for removing divalent metal ions, but Na type adsorption is generally needed, or the pH value environment of feed liquid is higher, so that the adsorption effect on divalent ions in an acidic system is very limited. Through a large number of experimental screening, it is found that the amino carboxylic acid chelating resin or the amino phosphoric acid chelating resin can effectively adsorb calcium and magnesium ions.
In the step C, the weight percentage concentration of the acid liquor is 5-10%, and the weight percentage concentration of the alkali liquor is 5-10%.
In the step C, the acid liquid is one or a mixture of hydrochloric acid and sulfuric acid solution, and the alkali liquid is sodium hydroxide solution.
The step E of adding ethanol for dissolution refers to adding 1-1.5 times of ethanol into the dehydrated concentrated solution for dissolution. The weight percentage concentration of the ethanol is more than 99 percent. The final temperature of the cooling crystallization needs to reach 3-5 ℃. In order to overcome the defect that a large amount of ethanol is needed for crystallization of D-ribose, experiments prove that the water in the concentrated solution is key to influencing the use amount of the ethanol, and the residual water can cause the solubility of the D-ribose to be increased, so that the crystallization yield is low, and the yield is generally improved by adopting a method for increasing the ethanol. According to the method, the principle of azeotropy of ethanol and water is utilized, when no obvious water flows out of the concentrated solution, one time of ethanol with the mass concentration of 99% is added, after the ethanol is concentrated and recovered, the rest concentrated solution is almost anhydrous, 1-1.5 times of ethanol with the mass concentration of 99% is added into the concentrated solution, the temperature is reduced, crystallization and separation are carried out, and the filter cake is D-ribose.
Compared with the prior art, the invention is based on the process of hydrolyzing the adenosine by inorganic acid (hydrochloric acid and sulfuric acid), and the component detection is carried out on adenine mother liquor after adenine is separated, and the mother liquor is found to contain D-ribose, sodium chloride (or sodium sulfate), adenine, adenosine, protein, pigment and the like, wherein the D-ribose, the sodium chloride (or sodium sulfate) are mainly used. The invention separates and purifies the mother liquor, uses the mother liquor as a resource, obtains D-ribose, converts sodium chloride (or sodium sulfate) into acid liquor and alkali liquor, and recycles the acid liquor and alkali liquor to the processes of hydrolyzing adenosine and neutralizing, thereby realizing the recovery of D-ribose in adenine mother liquor and the effective utilization of acid-base circulation. The invention skillfully combines the bipolar membrane and the electrodialysis, not only removes inorganic salt in filtrate, but also converts the inorganic salt into acid liquor and alkali liquor. H between cathode and anode film composite layers under the action of direct current electric field by utilizing bipolar film 2 O dissociates into H + And OH (OH) - And pass through the negative film and the positive film respectively as H + And OH (OH) - Ion source, inorganic salt anion and cation ion ionized from filtrate in salt chamber pass through anion and cation exchange membrane and are respectively connected with H in acid chamber + And OH in the alkaline chamber - The ion source forms acid liquor and alkali liquor. Inorganic salt in the solution is converted into acid liquor and alkali liquor, and the acid liquor and the alkali liquor are recycled into the process, so that the investment of fresh acid-alkali raw materials is reduced, and meanwhile, the added value of inorganic salt byproducts is improved. The inorganic salt content of the salt chamber solution treated by the bipolar membrane is greatly reduced, residual inorganic salt is further enriched into concentrated brine by utilizing electrodialysis under the action of an electric field and is recycled to the bipolar membrane salt chamber, the desalted solution after electrodialysis is D-ribose solution, the salt content is reduced, and a qualified D-ribose product can be obtained through subsequent procedures. The invention obtains acid-base and D-ribose after the adenine mother liquor is treated, and utilizes the production waste as a resource, thereby being environment-friendly and increasing the economic benefit of enterprises.
Detailed Description
The method is environment-friendly, increases economic benefit, and overcomes the defects of difficult resource utilization and difficult environment-friendly treatment in the prior art. The present invention will be described in more detail by way of examples. However, the following examples are merely illustrative examples for the purpose of describing the present invention in detail, and the scope of the present invention is not limited to these examples.
Example 1
Taking 20L of adenine mother liquor (containing D-ribose and sodium chloride), adding 100mL of polyacrylamide solution with the concentration of 0.2% under the stirring condition, adjusting the pH value to 6.3, adding 100g of powdery active carbon at the temperature of 65 ℃, stirring for 25min, filtering, allowing filtrate to flow through a glass column filled with 1L of amino carboxylic acid chelate resin, adsorbing and separating calcium and magnesium ions in the filtrate, adding a resin collecting liquid into a bipolar membrane system for treatment, continuously circulating acid liquor, alkali liquor and collecting liquid respectively, stopping bipolar membrane treatment when the conductivity of the collecting liquid is reduced to 3.5mS/cm, obtaining 5.0L of hydrochloric acid solution with the concentration of 7.31%, and 5.5L of sodium hydroxide solution with the concentration of 7.21%, wherein the hydrochloric acid solution is returned to a preparation tank as acid and water for adenine mother liquor production, the sodium hydroxide solution is returned to a preparation tank as water for tablet alkali dissolution, preparing and then used for the neutralization procedure of purine mother liquor production, simultaneously obtaining a dilute salt collecting liquid after bipolar membrane treatment, treating the dilute salt collecting liquid by electrodialysis, stopping the electrodialysis when the conductivity of the dilute salt collecting liquid reaches 78 mu S/cm, and stopping the electrodialysis when the conductivity of the dilute salt collecting liquid reaches the concentration of 78 mu S/cm, and adding the dilute salt solution into the bipolar membrane collecting liquid under the bipolar membrane system, and the water in the bipolar membrane system, and recycling the concentrated solution D, and the concentrated solution. Concentrating and dehydrating the D-ribose solution by using a concentrating furnace, adding 1 time of volume amount of ethanol when no obvious water flows out, continuously concentrating and dehydrating, collecting recovered ethanol containing water to obtain dehydrated concentrated solution, adding 1 time of volume amount of ethanol for dissolving, adding active carbon for decoloring and filtering, cooling and crystallizing the filtrate, and separating and drying the crystallized solution to obtain 786g of D-ribose crystals. The yield of hydrochloric acid was 92.30%, the yield of sodium hydroxide was 91.38%, and the yield of D-ribose was 87.45%.
Example 2
Taking 25L of adenine mother liquor (containing D-ribose and sodium chloride), adding 175mL of polyacrylamide solution with the concentration of 0.2% under the stirring condition, adjusting the pH value to 6.5, adding 150g of powdery active carbon, stirring for 30min, adding 75g of diatomite, stirring and filtering, allowing filtrate to flow through a glass column filled with 1.25L of amino phosphoric acid chelate resin, adsorbing and separating calcium and magnesium ions in the filtrate, adding a resin collecting liquid into a bipolar membrane system for treatment, continuously circulating acid liquor, alkali liquor and collecting liquid respectively, stopping bipolar membrane treatment when the conductivity of the collecting liquid is reduced to 3.3mS/cm, obtaining 6.5L of hydrochloric acid solution, 7.0L of sodium hydroxide solution, and obtaining 6.85L of sodium hydroxide solution, wherein the hydrochloric acid solution is returned to a batching tank as acid and water for adenine mother liquor production, the sodium hydroxide solution is returned to an alkaline tank as water for tablet alkali dissolution, preparing and then using the process for purine mother liquor production, simultaneously obtaining dilute salt collecting liquid after bipolar membrane treatment, treating the dilute salt collecting liquid by electrodialysis, stopping the electric conductivity of the dilute salt collecting liquid to reach 85 mu S/cm, and adding the dilute salt collecting liquid into a bipolar membrane system under the desalination membrane, and obtaining the concentrated solution D-ribose by the bipolar membrane, and recovering the concentrated solution in the bipolar membrane D-ribose collecting liquid by the bipolar membrane. Concentrating and dehydrating the D-ribose solution by using a concentrating furnace, adding 1 time of volume amount of ethanol when no obvious water flows out, continuously concentrating and dehydrating, collecting recovered ethanol containing water to obtain dehydrated concentrated solution, adding 1.2 times of volume amount of ethanol for dissolving, adding active carbon for decoloring and filtering, cooling and crystallizing the filtrate, and separating and drying the crystallized solution to obtain 932g of D-ribose crystals. The yield of hydrochloric acid was 89.82%, the yield of sodium hydroxide was 88.39%, and the yield of D-ribose was 82.95%.
Example 3
Taking 20L of adenine mother liquor (containing D-ribose and sodium chloride), adding 200mL of polyacrylamide solution with the concentration of 0.2% under the stirring condition, adjusting the pH value to 6.8, adding 110g of powdery active carbon, stirring for 35min, filtering, allowing filtrate to flow through a glass column filled with 1L of amino phosphoric acid chelate resin, adsorbing and separating calcium and magnesium ions in the filtrate, adding a resin collecting liquid into a bipolar membrane system for treatment, continuously circulating acid liquor, alkali liquor and collecting liquid respectively, stopping bipolar membrane treatment when the conductivity of the collecting liquid is reduced to 3.0mS/cm, obtaining 5.0L of hydrochloric acid solution with the concentration of 7.15%, and 5.5L of sodium hydroxide solution with the concentration of 7.14%, wherein the hydrochloric acid solution is returned to a preparation tank as acid and water for adenine mother liquor production, the sodium hydroxide solution is returned to a preparation tank as water for tablet alkali dissolution, preparing and then used for the neutralization procedure of purine mother liquor production, simultaneously obtaining a dilute salt collecting liquid after bipolar membrane treatment, treating the dilute salt collecting liquid by electrodialysis, stopping the electrodialysis when the conductivity of the dilute salt collecting liquid reaches 73 mu S/cm, obtaining the brine and the concentrated solution, and the brine solution under the bipolar membrane system is added into the bipolar membrane system for water recovery when the conductivity of the concentrated solution D is desalinated by the bipolar membrane. Concentrating and dehydrating the D-ribose solution by using a concentrating furnace, adding 1 time of volume amount of ethanol when no obvious water flows out, continuously concentrating and dehydrating, collecting recovered ethanol containing water to obtain dehydrated concentrated solution, adding 1.5 times of volume amount of ethanol for dissolving, adding active carbon for decoloring and filtering, cooling and crystallizing the filtrate, and separating and drying the crystallized solution to obtain 795g of D-ribose crystals. The yield of hydrochloric acid was 90.28%, the yield of sodium hydroxide was 90.49%, and the yield of D-ribose was 88.45%.
Example 4
Taking 20L of adenine mother liquor (containing D-ribose and sodium sulfate), adding 120mL of polyacrylamide solution with the concentration of 0.2 percent under the stirring condition, adjusting the pH value to 6.5, adding 110g of powdery active carbon, stirring for 30min, adding 100g of diatomite, stirring and filtering, allowing filtrate to flow through a glass column filled with 1L of amino carboxylic acid chelate resin, adsorbing and separating calcium and magnesium ions in the filtrate, adding a resin collecting liquid into a bipolar membrane system for treatment, continuously circulating acid liquor, alkali liquor and collecting liquid respectively, stopping bipolar membrane treatment when the conductivity of the collecting liquid is reduced to 3.2mS/cm, obtaining 6.0L of sulfuric acid solution with the concentration of 8.52 percent, and 6.0L of sodium hydroxide solution with the concentration of 7.28 percent, wherein the sulfuric acid solution is returned to a preparation tank as acid and water for producing adenine mother liquor, the sodium hydroxide solution is returned to an alkali preparation tank as water for dissolving tablets, preparing and then used for the neutralization procedure of producing purine mother liquor, simultaneously obtaining a dilute salt collecting liquid after bipolar membrane treatment, carrying out electrodialysis treatment on the dilute salt collecting liquid, stopping the dilute salt collecting liquid until the conductivity of 55 mu S/cm, stopping the electric conductivity of the dilute salt collecting liquid reaches the bipolar membrane, and desalting the dilute salt collecting liquid, and obtaining the dilute salt solution, and the water under the bipolar membrane D, and desalting the aqueous solution, and the concentrated solution, and the aqueous solution is recovered by the bipolar membrane D in the bipolar membrane system. Concentrating and dehydrating the D-ribose solution by using a concentrating furnace, adding 1 time of volume amount of ethanol when no obvious water flows out, continuously concentrating and dehydrating, collecting recovered ethanol containing water to obtain dehydrated concentrated solution, adding 1.2 times of volume amount of ethanol for dissolving, adding active carbon for decoloring and filtering, cooling and crystallizing the filtrate, and separating and drying the crystallized solution to obtain 768g of D-ribose crystals. The sulfuric acid yield was 86.94%, the sodium hydroxide yield was 91.07%, and the D-ribose yield was 85.44%.
Example 5
Taking 25L of adenine mother liquor (containing D-ribose and sodium sulfate), adding 200mL of polyacrylamide solution with the concentration of 0.2% under the stirring condition, adjusting the pH value to 6.8, adding 150g of powdery active carbon, stirring for 35min, filtering, allowing filtrate to flow through a glass column filled with 1.25L of amino phosphoric acid chelate resin, adsorbing and separating calcium and magnesium ions in the filtrate, adding a resin collecting liquid into a bipolar membrane system for treatment, continuously circulating acid liquor, alkali liquor and collecting liquid respectively, stopping bipolar membrane treatment when the conductivity of the collecting liquid is reduced to 3.4mS/cm, obtaining 7.5L of sulfuric acid solution with the concentration of 8.33%, and 7.5L of sodium hydroxide solution with the concentration of 7.16%, wherein the sulfuric acid solution is returned to a preparation tank as acid and water for adenine mother liquor production, the sodium hydroxide solution is returned to an alkali preparation tank as water for sheet alkali dissolution, preparing and then used for the neutralization procedure of purine mother liquor production, simultaneously obtaining a dilute salt collecting liquid after bipolar membrane treatment, treating the dilute salt collecting liquid by electrodialysis, stopping the electrodialysis when the conductivity of the dilute salt collecting liquid reaches 65 mu S/cm, and obtaining the brine and the aqueous solution under the bipolar membrane system, and adding the dilute salt collecting liquid into the bipolar membrane system for desalting the water and the aqueous solution under the bipolar membrane system, and recovering the aqueous solution from the ribose-D. Concentrating and dehydrating the D-ribose solution by using a concentrating furnace, adding 1 time of volume amount of ethanol when no obvious water flows out, continuously concentrating and dehydrating, collecting recovered ethanol containing water to obtain dehydrated concentrated solution, adding 1.5 times of volume amount of ethanol for dissolving, adding active carbon for decoloring and filtering, cooling and crystallizing the filtrate, and separating and drying the crystallized solution to obtain 985g of D-ribose crystals. The sulfuric acid yield was 85.00%, the sodium hydroxide yield was 89.57%, and the D-ribose yield was 87.67%.
The main data of the above embodiment are listed as follows:
in the above examples 1-5, the adenine mother liquor was treated to obtain acid-base and D-ribose, the acid-base was recycled, the D-ribose was formed into a product, and the acid liquor, alkali liquor and D-ribose were all obtained in high yields. Namely, the production waste is recycled, which is environment-friendly and increases the economic benefit of enterprises.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (10)
1. A method for producing D-ribose and recycling acid and alkali by adenine mother liquor comprises the following steps:
A. adding polyacrylamide solution into adenine mother liquor for pretreatment, regulating pH to 6.0-7.0, regulating temperature to 60-70 ℃, adding active carbon to decolorize the adenine mother liquor, stirring for 25-35min, and filtering to obtain clear filtrate;
B. allowing the filtrate obtained in the step A to flow through a chelating resin column, and adsorbing and separating calcium and magnesium ions in the filtrate to obtain clarified collecting liquid;
C. b, treating the collecting liquid in the step B by using a bipolar membrane to obtain an acid liquid, an alkali liquid and a dilute salt collecting liquid; the conductivity of the dilute salt collecting solution is reduced to 3-3.5mS/cm, and bipolar membrane treatment is stopped; the acid liquor returns to the batching tank to be used as acid and water for adenine mother liquor production; the alkali liquor returns to the alkali distribution tank to be used as water for dissolving the flake alkali and is used for neutralization during the production of adenine mother liquor;
D. treating the dilute salt collecting liquid in the step C by electrodialysis, stopping electrodialysis when the conductivity of the dilute salt collecting liquid reaches 50-100 mu S/cm to obtain desalted liquid and concentrated brine, wherein the desalted liquid is D-ribose solution, and the concentrated brine returns to the step C and is mixed with the collecting liquid in the step B, and treating by a bipolar membrane;
E. and D-ribose solution in the step D is concentrated and dehydrated by a concentration furnace, when no obvious water flows out, ethanol with volume of one time is added, the concentration and dehydration are continued, the recovered ethanol containing water is collected, the dehydrated concentrated solution is obtained, and then ethanol is added for dissolution, activated carbon is added for decoloration, filtration, cooling crystallization, separation and drying are carried out, so that D-ribose crystals are obtained.
2. The method for producing D-ribose and recycling acid and alkali by adenine mother liquor according to claim 1, wherein the method comprises the following steps: the addition amount of the polyacrylamide solution in the step A is 0.5-1.0% of the volume percentage of the adenine mother solution.
3. The method for producing D-ribose and recycling acid and alkali by adenine mother liquor according to claim 2, wherein the method comprises the following steps: the weight percentage concentration of the polyacrylamide solution is 0.2%.
4. The method for producing D-ribose and recycling acid and alkali by using adenine mother liquor to produce adenine mother liquor according to claim 3, wherein the method comprises the following steps: the addition amount of the activated carbon in the step A is 0.50-0.65% of the volume percentage of the adenine mother solution.
5. The method for producing D-ribose and recycling acid and alkali by adenine mother liquor according to claim 1, wherein the method comprises the following steps: the chelating resin in the step B is amino carboxylic acid chelating resin or amino phosphoric acid chelating resin.
6. The method for producing D-ribose and recycling acid and alkali by adenine mother liquor according to claim 1, wherein the method comprises the following steps: in the step C, the weight percentage concentration of the acid liquor is 5-10%, and the weight percentage concentration of the alkali liquor is 5-10%.
7. The method for producing D-ribose and recycling acid and alkali by adenine mother liquor according to claim 1, wherein the method comprises the following steps: in the step C, the acid liquid is one or a mixture of hydrochloric acid and sulfuric acid solution, and the alkali liquid is sodium hydroxide solution.
8. The method for producing D-ribose and recycling acid and alkali by adenine mother liquor according to claim 1, wherein the method comprises the following steps: the step E of adding ethanol for dissolution refers to adding 1-1.5 times of ethanol into the dehydrated concentrated solution for dissolution.
9. The method for producing D-ribose and recycling acid and alkali by adenine mother liquor according to claim 1 or 8, wherein the method comprises the following steps: the weight percentage concentration of the ethanol is more than 99 percent.
10. The method for producing D-ribose and recycling acid and alkali by adenine mother liquor according to claim 9, wherein the method comprises the following steps: the final temperature of the cooling crystallization needs to reach 3-5 ℃.
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