CN106220520B - A kind of processing method of beet alkali hydrochlorate calcium method production technology waste liquor - Google Patents
A kind of processing method of beet alkali hydrochlorate calcium method production technology waste liquor Download PDFInfo
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- CN106220520B CN106220520B CN201610629991.9A CN201610629991A CN106220520B CN 106220520 B CN106220520 B CN 106220520B CN 201610629991 A CN201610629991 A CN 201610629991A CN 106220520 B CN106220520 B CN 106220520B
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- beet alkali
- alkali hydrochlorate
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/38—Separation; Purification; Stabilisation; Use of additives
- C07C227/40—Separation; Purification
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/38—Separation; Purification; Stabilisation; Use of additives
- C07C227/40—Separation; Purification
- C07C227/42—Crystallisation
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Abstract
The invention discloses a kind of processing method of beet alkali hydrochlorate calcium method production technology waste liquor, belong to liquid waste disposal technique field, this method includes into the waste liquor of calcium method production technology plus water heating, adjusts pH value of solution with calcium hydroxide, catches up with except alkaline gas, cooling carries out separation of solid and liquid, sulfuric acid is added in the stillness of night, again separation of solid and liquid, hydrochloric acid is added in the stillness of night, decrease temperature crystalline, separation of solid and liquid obtain product beet alkali hydrochlorate.This method cost is cheap, reaction relaxes, it is low for equipment requirements, processed beet alkali hydrochlorate calcium method synthesis technique waste liquor, easily can go out most product through being dehydrated Crystallization Separation, or can directly apply mechanically go back to beet alkali hydrochlorate calcium method synthesis technique dehydration workshop section, the rate of recovery more than 78% of beet alkali hydrochlorate in mother liquor, it is cost-effective with stronger operability, greatly improve the economic benefit of enterprise.
Description
Technical field
The invention belongs to liquid waste disposal technique field, more particularly to a kind of beet alkali hydrochlorate calcium method production technology waste liquor
Processing method.
Background technology
Beet alkali hydrochlorate also known as betaine HCL, trimethylglycine hydrochloride, are a kind of efficient, high-quality, economical, wide
It is general applied to poultry, fowl, aquaculture food attractant-growth promoting auxotype additive.
Beet alkali hydrochlorate calcium method synthesis technique, calcium chloroacetate, monoxone are obtained using monoxone and calcium hydroxide reaction
Calcium reacts to obtain the mixture of glycine betaine and calcium chloride with trimethylamine, adds separating calcium sulphate after sulfuric acid, and feed liquid is crystallized through dehydration
Beet alkali hydrochlorate is obtained, specific reaction equation is as follows：
The final waste liquor of the technique, after multiple condensing crystallizing, it may appear that color blackening, viscosity increase, is non crystallized
Situation, although product beet alkali hydrochlorate content is more than 20wt% in the waste liquor, it is difficult to product is separated, and
Mother liquid recycle can not be carried out, otherwise can influence reaction yield.Under normal conditions, which can only carry out waste treatment.
Application No. 201210307259.1, a kind of entitled patent application of the preparation method of beet alkali hydrochlorate
Disclose and " make the catalyst of nucleophilic displacement of fluorine with sodium iodide, first carry out under catalyst action trimethylamine with monoxone quaternary ammoniated
Reaction, then adds calcium oxide or calcium hydroxide, heats up and trimethylamine is emptied, after with sulfuric acid be acidified to obtain calcium sulfate and beet alkali salt
Acid salt solution, reaction solution is filtered, concentrate, crystallization obtains the technical solution of beet alkali hydrochlorate ", described in the patent application
Method is processing to reaction solution, due to the difference on the component in reaction solution and waste liquor, e.g., trimethylamine in waste liquor with
And the content of acid soluble impurities is significantly higher than reaction solution, therefore, such a method is not suitable for handling waste liquor.
The content of the invention
The present invention in the prior art the defects of to provide a kind of cost cheap, reaction relaxes, and can be readily separated sweet tea
Product and the high beet alkali hydrochlorate calcium method production technology waste liquor of the rate of recovery in dish alkali salt hydrochlorate calcium method synthesis technique waste liquor
Processing method.
The principle of the invention：Inventor is found through experiments that, in beet alkali hydrochlorate calcium method synthesis technique waste liquor, influences to produce
The factor of product crystallization includes following three points：
(1) trimethylamine excessive in product building-up process is retained in mother liquor after sulfuric acid reaction in the form of front three amine salt
In；
(2) acid soluble impurities in raw material calcium hydroxide during the reaction, are exported into solution system and not, entirely
Portion is accumulated into mother liquor；
(3) the water-soluble byproduct of reaction is stayed in mother liquor always.
In order to achieve the object of the present invention, the technical scheme is that：
A kind of processing method of beet alkali hydrochlorate calcium method production technology waste liquor, into the waste liquor of calcium method production technology
Add water to heat up, pH value of solution is adjusted with calcium hydroxide, catch up with except alkaline gas, cooling carry out separation of solid and liquid, sulfuric acid added in the stillness of night, then
Secondary separation of solid and liquid, adds hydrochloric acid, decrease temperature crystalline in the stillness of night, separation of solid and liquid obtains product beet alkali hydrochlorate.
The present invention also has following additional technical feature：
Preferably, comprise the following steps：
Step 1. by the waste liquor of beet alkali hydrochlorate calcium method production technology add etc. weight water, be warming up to 70 DEG C；
Step 2. is slowly added to calcium hydroxide, adjustment pH value of solution to 10-12；
Step 3. adds the sodium hydrate solid of ‰ -0.5wt ‰ of waste liquor gross weight 0.25wt as auxiliary agent；
Step 4. is kept for 65 DEG C -85 DEG C catch up with except alkaline gas, keeps system pH=10-11, pH to use calcium hydroxide after reducing
Adjustment, untill gas phase pH=7 is exported；
Step 5. is cooled to less than 40 DEG C, and separation of solid and liquid is carried out by settling centrifugal process；
The sulfuric acid for the calcium hydroxide equimolar number for adding and using in the clear liquid of step 6. separation of solid and liquid, separation of solid and liquid generation
Calcium sulfate；
After step 7. separates the suitable water of clear liquid abjection of calcium sulfate, add waste liquor gross weight 3wt%-5wt%'s
Hydrochloric acid obtains product beet alkali hydrochlorate as Crystallization Separation auxiliary agent, decrease temperature crystalline, separation of solid and liquid.
Preferably, the waste liquor is that sulfuric acid is acidified, mistake filters out according to the reaction solution of calcium chloroacetate and trimethylamine is added
Go obtained by the method for calcium sulfate, filtrate through decrease temperature crystalline several times.
Preferably, pH value of solution is adjusted in the step 2 to 10-11.
Preferably, in the step 3 sodium hydroxide addition be waste liquor gross weight 0.25wt ‰.
Preferably, the temperature control except alkaline gas is caught up with the step 4 at 70-75 DEG C.
Preferably, separation of solid and liquid removes impurity and uses sedimentation centrifuge in the step 5.
Preferably, the auxiliary agent of Crystallization Separation is that mass fraction is 31% concentrated hydrochloric acid in the step 7, and addition is waste liquor
The 3wt% of gross weight.
Experimental analysis：The difference of waste liquor and reaction solution component：
(1) amine compounds containing front three：Contain micro amination containing front three in beet alkali hydrochlorate calcium method synthesis reaction solution
Compound, these amine compounds containing front three are with trimethylamine hydrochloride, existing for metal trimethylamine complex form.Contain in reaction solution
Trimethylamine compounds content usually≤0.05wt% in terms of trimethylamine, this part amine compounds containing front three only has≤and 20wt% can be with
The crystallization of product beet alkali hydrochlorate separates out, remaining to fully enter mother liquor, and progressively adds up with applying mechanically for mother liquor.It is final useless
Compounds content containing trimethylamine can exceed 2wt% in terms of trimethylamine in mother liquor；Traditional beet alkali hydrochlorate calcium method synthesis technique
In, the trimethylamine processing mode of use is only to add calcium hydroxide to discharge trimethylamine, because the solubility of calcium hydroxide in itself
Problem, causes system basicity not strong enough, be only capable of divided by trimethylamine hydrochloride form existing for amine compounds containing front three, and metal
Trimethylamine in front three amine complex can not discharge, therefore use this method, to the amine compounds containing front three in processing waste liquor
Thing effect is very limited.
(2) acid soluble impurities：Containing with the presence of a small amount of acid soluble impurities in beet alkali hydrochlorate calcium method synthesis reaction solution,
This partial impurities includes silicate, the calcium ions and magnesium ions brought by raw material calcium hydroxide, and in beet alkali hydrochlorate building-up process
Hydroxyacetic acid and its derivative of generation etc..Acid soluble impurities content in reaction solution is usually reaction solution (quaternization process)
When the 0.4wt% of weight, pH≤4, acid soluble impurities are fully dissolved in system, and will not be with product beet alkali hydrochlorate knot
Partial crystallization goes out, because reaction solution pH ＜ 2 when beet alkali hydrochlorate crystallizes, acid soluble impurities are remained in mother liquor always, and with
Applying mechanically for mother liquor progressively to add up, when acid soluble impurities ratio exceedes the 10wt% of mother liquor weight, even if beet alkali hydrochlorate
Reach supersaturation and be also very difficult to crystallization, mother liquor can only waste treatment；In beet alkali hydrochlorate calcium method synthesis technique, crystalline mother solution
Be set use dehydration crystallisation step, the pH ＜ 2 of system, acid soluble impurities can not separate out completely at this time, thus this partial impurities without
Method is handled.
Beneficial effects of the present invention are：This method cost is cheap, and reaction relaxes, low for equipment requirements, processed beet
Alkali salt hydrochlorate calcium method synthesis technique waste liquor, easily can go out most product through being dehydrated Crystallization Separation, or can be with
Directly apply mechanically back beet alkali hydrochlorate calcium method synthesis technique and be dehydrated workshop section, in mother liquor the rate of recovery 78% of beet alkali hydrochlorate with
On, there is stronger operability, it is cost-effective, greatly improve the economic benefit of enterprise.
The additional aspect and advantage of the present invention will be set forth in part in the description, and will partly become from the following description
Obtain substantially, or recognized by the practice of the present invention.
Embodiment
The embodiment of the present invention is described below in detail, wherein same or similar label represents same or like from beginning to end
Element or there is same or like element.The following examples are exemplary, it is intended to for explaining the present invention, and
It is not considered as limiting the invention.Below in conjunction with instantiation, the present invention is described in detail.
Embodiment 1
It will be added in 1000g beet alkali hydrochlorate calcium method synthesis waste liquor (beet alkali hydrochlorate content 29.3wt%)
1000g water, is warming up to 70 DEG C, stirs the lower calcium hydroxide that adds to the pH=10 of solution, adds 0.25g sodium hydroxides, keep molten
Liquid temperature degree and pH value, until outlet gas phase pH=7, shares calcium hydroxide (92wt%) 77.8g；
Less than 40 DEG C are cooled to, insoluble impurity is removed by sedimentation centrifuge separation of solid and liquid；
The clear liquid of separation of solid and liquid adds 96.7g sulfuric acid (98wt%), filters the calcium sulfate for removing generation；
Filtrate decompression is dehydrated to a large amount of crystallizations, is added 30g hydrochloric acid (31wt%), is cooled to 30 DEG C once, and suction filtration is produced
Product beet alkali hydrochlorate 230.1g, product recovery rate 78.5%.
Embodiment 2
2000kg beet alkali hydrochlorate calcium method synthesis waste liquor (beet alkali hydrochlorate content is put into reaction kettle
30.1wt%) with 2000kg water, 73 DEG C are warming up to, the lower industrial goods calcium hydroxide that adds is stirred to pH value of solution=11, adds 0.5kg
Sodium hydroxide, keeps 70-75 DEG C of temperature in the kettle, keeps material liquid pH=10-11 in kettle, until gas phase pipe outlet pH=7, shares hydrogen
Calcium oxide (92.2wt%) 161kg；
It is cooled to 40 DEG C once, insoluble impurity is removed by sedimentation centrifuge separation of solid and liquid；
Separation of solid and liquid clear liquid adds the 206.6kg industrial goods concentrated sulfuric acid (93wt%), and the sulfuric acid of generation is removed by centrifuge
Calcium；
Filtrate decompression is dehydrated to a large amount of crystallizations, adds 60kg concentrated hydrochloric acids (31wt%), is cooled to 30 DEG C, centrifugation obtains product
Beet alkali hydrochlorate 476kg, product recovery rate 79.3%.
Comparative example 1
Traditional handicraft：
1000g beet alkali hydrochlorate calcium method is synthesized into waste liquor (beet alkali hydrochlorate content 28.4wt%, trimethylamine content
1000g water is added in 2.3wt%), is warming up to 70 DEG C, the lower calcium hydroxide that adds is stirred to pH value of solution=10, keeps solution temperature
With pH value, until exporting gas phase pH=7, calcium hydroxide (92wt%) 76.2g is shared.React and system is acidified to pH ＜ 2, altogether
Solution 2316g is obtained, trimethylamine content 0.807%, the removal rate of trimethylamine is 18.7%.
Less than 40 DEG C are cooled to, adds 94.7g sulfuric acid (98wt%), filters the calcium sulfate for removing generation.
Decompression dehydration is cooled to 30 DEG C, crystallizes and separate out without beet alkali hydrochlorate to remaining 710g.Continue dehydration to residue
550g, is cooled to 30 DEG C, and system becomes very sticky, there is a small amount of beet alkali hydrochlorate crystal in liquid, but can not solid-liquid point
From.
The technique of the present invention：
1000g beet alkali hydrochlorate calcium method is synthesized into waste liquor (beet alkali hydrochlorate content 28.4wt%, trimethylamine content
1000g water is added in 2.3wt%), is warming up to 70 DEG C, the lower calcium hydroxide that adds is stirred to pH value of solution=10, adds 0.25g hydrogen-oxygens
Change sodium, keep solution temperature and pH value, until outlet gas phase pH=7, shares calcium hydroxide (92wt%) 75.5g.Having reacted will
System is acidified to pH ＜ 2, there are solution 2297g, trimethylamine content 0.011%, the removal rate of trimethylamine is 98.9%.
Less than 40 DEG C are cooled to, insoluble impurity is removed by sedimentation centrifuge separation of solid and liquid.
The clear liquid of separation of solid and liquid adds 94.2g sulfuric acid (98wt%), filters the calcium sulfate for removing generation.
Filtrate decompression is dehydrated to a large amount of crystallizations, adds 30g hydrochloric acid (31wt%), is cooled to less than 30 DEG C, suction filtration is produced
Product beet alkali hydrochlorate 224.4g, product recovery rate 79.0%.
In the description of this specification, reference term " one embodiment ", " some embodiments ", " example ", " specifically show
The description of example " or " some examples " etc. means specific features, structure, material or the spy for combining the embodiment or example description
Point is contained at least one embodiment of the present invention or example.In the present specification, schematic expression of the above terms is not
It must be directed to identical embodiment or example.Moreover, particular features, structures, materials, or characteristics described can be in office
What combined in an appropriate manner in one or more embodiments or example.In addition, those skilled in the art can say this
Different embodiments or example described in bright book are engaged and combined.
Although an embodiment of the present invention has been shown and described, it will be understood by those skilled in the art that：Not
In the case of departing from the principle of the present invention and objective a variety of change, modification, replacement and modification can be carried out to these embodiments, this
The scope of invention is limited by claim and its equivalent.
Claims (8)
1. a kind of processing method of beet alkali hydrochlorate calcium method production technology waste liquor, it is characterised in that to calcium method production technology
Waste liquor in plus water heating, adjust pH value of solution with calcium hydroxide, add the hydrogen of ‰ -0.5wt ‰ of waste liquor gross weight 0.25wt
Sodium oxide molybdena solid is caught up with except alkaline gas, cooling carry out separation of solid and liquid, sulfuric acid added in the stillness of night, again separation of solid and liquid as auxiliary agent,
Hydrochloric acid, decrease temperature crystalline are added in the stillness of night, separation of solid and liquid obtains product beet alkali hydrochlorate.
2. the processing method of beet alkali hydrochlorate calcium method production technology waste liquor according to claim 1, it is characterised in that
Comprise the following steps：
Step 1. by the waste liquor of beet alkali hydrochlorate calcium method production technology add etc. weight water, be warming up to 70 DEG C；
Step 2. is slowly added to calcium hydroxide, adjustment pH value of solution to 10-12；
Step 3. adds the sodium hydrate solid of ‰ -0.5wt ‰ of waste liquor gross weight 0.25wt as auxiliary agent；
Step 4. is kept for 65 DEG C -85 DEG C catch up with except alkaline gas, is adjusted after keeping system pH=10-11, pH reduction with calcium hydroxide,
Untill outlet gas phase pH=7；
Step 5. is cooled to less than 40 DEG C, and separation of solid and liquid is carried out by settling centrifugal process；
The sulfuric acid for the calcium hydroxide equimolar number for adding and using in the clear liquid of step 6. separation of solid and liquid, the sulphur of separation of solid and liquid generation
Sour calcium；
After step 7. separates the suitable water of clear liquid abjection of calcium sulfate, the hydrochloric acid for adding waste liquor gross weight 3wt%-5wt% is made
For Crystallization Separation auxiliary agent, decrease temperature crystalline, separation of solid and liquid obtains product beet alkali hydrochlorate.
3. the processing method of beet alkali hydrochlorate calcium method production technology waste liquor according to claim 1 or 2, its feature exist
In, the waste liquor be according to the reaction solution of calcium chloroacetate and trimethylamine is added sulfuric acid acidifying, is filtered to remove calcium sulfate, filtrate
Obtained by method through decrease temperature crystalline several times.
4. the processing method of beet alkali hydrochlorate calcium method production technology waste liquor according to claim 2, it is characterised in that
PH value of solution is adjusted in the step 2 to 10-11.
5. the processing method of beet alkali hydrochlorate calcium method production technology waste liquor according to claim 2, it is characterised in that
The addition of sodium hydroxide is the 0.25wt ‰ of waste liquor gross weight in the step 3.
6. the processing method of beet alkali hydrochlorate calcium method production technology waste liquor according to claim 2, it is characterised in that
The temperature control except alkaline gas is caught up with the step 4 at 70-75 DEG C.
7. the processing method of beet alkali hydrochlorate calcium method production technology waste liquor according to claim 2, it is characterised in that
Separation of solid and liquid removes impurity and uses sedimentation centrifuge in the step 5.
8. the processing method of beet alkali hydrochlorate calcium method production technology waste liquor according to claim 2, it is characterised in that
The auxiliary agent of Crystallization Separation is that mass fraction is 31% concentrated hydrochloric acid in the step 7, and addition is the 3wt% of waste liquor gross weight.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103524364A (en) * | 2013-10-22 | 2014-01-22 | 潍坊祥维斯化学品有限公司 | Trimethylglycine hydrochloride mother liquor treatment process |
| CN105367432A (en) * | 2015-12-02 | 2016-03-02 | 山东祥维斯生物科技股份有限公司 | Method for preparing calcium method betaine |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103524364A (en) * | 2013-10-22 | 2014-01-22 | 潍坊祥维斯化学品有限公司 | Trimethylglycine hydrochloride mother liquor treatment process |
| CN105367432A (en) * | 2015-12-02 | 2016-03-02 | 山东祥维斯生物科技股份有限公司 | Method for preparing calcium method betaine |
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Application publication date: 20161214 Assignee: Jinan IFT Science & Technology Co., Ltd. Assignor: Chemical Inst., Shandong Prov. Contract record no.: 2018370000038 Denomination of invention: Method for treating waste mother liquor in calcium-based method production process of betaine hydrochloride Granted publication date: 20180515 License type: Common License Record date: 20180907 |