CN108440321A - A method of processing beet alkali hydrochlorate sodium method production technology waste liquor - Google Patents
A method of processing beet alkali hydrochlorate sodium method production technology waste liquor Download PDFInfo
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- CN108440321A CN108440321A CN201810378870.0A CN201810378870A CN108440321A CN 108440321 A CN108440321 A CN 108440321A CN 201810378870 A CN201810378870 A CN 201810378870A CN 108440321 A CN108440321 A CN 108440321A
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- waste liquor
- ethyl alcohol
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- beet alkali
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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
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/82—Purification; Separation; Stabilisation; Use of additives
- C07C209/86—Separation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A method of processing beet alkali hydrochlorate sodium method production technology waste liquor includes the following steps：Waste liquor is first used into naoh treatment recovery section trimethylamine；Reaction solution is concentrated again, absolute ethyl alcohol is added while hot, is filtered when stirring to room temperature, filtrate is distilled to recover ethyl alcohol.Method provided by the invention is easy to operate, it is of low cost, reaction is mild, low for equipment requirements, processed glycine betaine sodium method synthesis technology waste liquor, separation of solid and liquid can be easily achieved, the filter cake of the filter cake of the 55wt% of recyclable waste liquor amount, recycling can generate added value, and the ethyl alcohol used in the process can be recycled by way of distillation, it is cost-effective, there is larger economic value.
Description
Technical field
The present invention relates to glycine betaine technical field more particularly to a kind of useless mothers of processing beet alkali hydrochlorate sodium method production technology
The method of liquid.
Background technology
Beet alkali hydrochlorate is also known as betaine HCL, is that one kind is efficient, high-quality, economical, is widely used in poultry, fowl, aquatic products
The auxotype additive of the food attractant-growth promoting of cultivation.
Beet alkali hydrochlorate sodium method production technology is reacted with sodium hydroxide using monoxone and generates sodium chloroacetate, monoxone
Sodium is obtained by the reaction glycine betaine with trimethylamine and mixes completion liquid with sodium chloride, and after high temperature filters salt, hydrochloric acid is added, cools down, and filtering obtains
To beet alkali hydrochlorate.
Mother liquor is repeated caused by beet alkali hydrochlorate sodium method production technology applies mechanically, it may appear that color burn, viscosity increase
Big present situation can not be applied mechanically, become waste liquor again.After testing, main component is water, beet alkali hydrochlorate, sodium chloride, salt
Acid, trimethylamine hydrochloride, hydroxy acid sodium and other unknown materials.
Application No. is 201610629991.9, a kind of entitled beet alkali hydrochlorate calcium method production technology waste liquor
Processing method discloses and " adds water heating into the waste liquor of calcium method production technology, adjust pH value of solution with calcium hydroxide, catch up with except alkali
Property gas, cooling be separated by solid-liquid separation, sulfuric acid is added in clear liquid, is separated by solid-liquid separation again, hydrochloric acid is added in clear liquid, decrease temperature crystalline,
Separation of solid and liquid obtains product beet alkali hydrochlorate ", it is all the waste liquor for handling beet alkali hydrochlorate and generating, but production technology is calcium
Method, waste liquor ingredient differ, and the method is not suitable for handling the waste liquor that sodium method technique generates.
Therefore, a kind of method of new processing beet alkali hydrochlorate sodium method production technology waste liquor is developed, is not only had urgent
Researching value, it may have good economic benefit and commercial application potentiality, this is exactly where power for being accomplished of the present invention
The basis and.
Invention content
In order to overcome the defect of the prior art as indicated above, the present inventor to have made intensive studies this, paying
After a large amount of creative works, so as to complete the present invention.
Specifically, the technical problem to be solved by the present invention is to：A kind of processing beet alkali hydrochlorate sodium method production is provided
The method of technique waste liquor, to be suitable for beet alkali hydrochlorate process for producing sodium waste liquor, and also it is easy to operate, it is of low cost,
Reaction is mild.
In order to solve the above technical problems, the technical scheme is that：
A method of processing beet alkali hydrochlorate sodium method production technology waste liquor includes the following steps：By waste liquor elder generation
With naoh treatment recovery section trimethylamine；Reaction solution is concentrated again, absolute ethyl alcohol, stirring to mistake when room temperature are added while hot
Filter, filtrate are distilled to recover ethyl alcohol.
In the present invention, as a kind of perferred technical scheme, described method includes following steps：
(1) waste liquor is handled with a concentration of 30wt% sodium hydroxide solutions, and the rate for first pressing 20-25ml/s is added, later
It is added with the rate of 5-10ml/s, it is alkalescent that addition terminal, which is reaction solution pH, and the trimethylamine generated in the process is recycled；
(2) step (1) reaction solution is concentrated；
(3) absolute ethyl alcohol is added into concentrate obtained by step (2), filters, filter cake recycles；
(4) gained filtrate in step (3) is subjected to distillation processing, recycles ethyl alcohol.
In the present invention, as a kind of perferred technical scheme, the trimethylamine generated in the process is carried out with water in step (1)
Recycling.
In the present invention, as a kind of perferred technical scheme, waste liquor and the terminal of sodium hydroxide reaction are in step (1)
PH is 7.0-8.0.
In the present invention, as a kind of perferred technical scheme, reaction solution is in 95-100 DEG C of temperature, pressure in step (2)
0.07MPa, until being concentrated into bubble-free generation.
In the present invention, as a kind of perferred technical scheme, absolute ethyl alcohol is added in step (3) while hot, and stir, ethyl alcohol
Amount is 5wt% -25wt% of waste liquor amount.
In the present invention, as a kind of perferred technical scheme, in step (3) concentrate be 65-75 DEG C when be added it is anhydrous
During which ethyl alcohol opens stirring, stir speed (S.S.) 300-400rpm.
In the present invention, as a kind of perferred technical scheme, in step (3) when temperature is reduced to 20-25 DEG C, in vacuum
Degree filters under the conditions of being 0.07-0.09MPa.
In the present invention, as a kind of perferred technical scheme, steps are as follows for the method：
The waste liquor for weighing the synthesis of beet alkali hydrochlorate sodium method is placed in more mouthfuls of round-bottomed flasks, is first added by the rate of 20ml/s
Enter, the sodium hydroxide solution that a concentration of 30wt% is added with the rate of 5ml/s later to pH=7.5, use by the trimethylamine escaped
Water absorbs；
It is 100 DEG C to be heated to temperature, and under the conditions of vacuum degree 0.07MPa, stir speed (S.S.) is 400rpm stirring concentration 2h, concentration
Until bubble-free generates；
When temperature is down to 75 DEG C, absolute ethyl alcohol is added while hot, during which always on stirring, rate 400rpm；
When temperature is down to 20 DEG C, is filtered under the conditions of vacuum degree 0.07MPa, obtain filter cake, filtrate；
Filtrate is distilled, ethyl alcohol is recycled.
The present invention is directed to the difficult present situation of beet alkali hydrochlorate sodium method production technology waste liquor, provides a kind of operation letter
Just, of low cost, mild processing method is reacted, while reducing waste liquor reserves, the solid of recycling can recycle, and increase
Add economic value.
Inventor has found, in beet alkali hydrochlorate sodium method production process, because in reaction trimethylamine be it is excessive, because
This, excessive trimethylamine is reacted with hydrochloric acid in waste liquor is stored in the form of trimethylamine hydrochloride in mother liquor.And it is only a small amount of
Trimethylamine hydrochloride can be crystallized with beet alkali hydrochlorate and is precipitated, and lower batch of cycle can largely be entered with mother liquor, and with mother liquid recycle
The increase of number gradually adds up, and trimethylamine hydrochloride is unstable, and meeting lye can decompose, and with alkali neutralization reaction occurs for hydrochloric acid, puts
Heat, at this time most of trimethylamine can escape in gaseous form.
Inventor also found, in beet alkali hydrochlorate sodium method production process, monoxone as reaction raw materials, with hydrogen
Sodium oxide molybdena react generate sodium chloroacetate while, it is uncontrollable to generate a small amount of hydroxy acid sodium, due in acid condition
Under, hydroxy acid sodium is difficult to crystallize with beet alkali hydrochlorate and be precipitated, therefore, with applying mechanically for mother liquor, the content of hydroxy acid sodium
It can add up in mother liquor, when its ratio is more than 10wt%, beet alkali hydrochlorate reaching saturation is difficult to that crystallization is precipitated.
Based on considerations above, inventor realizes the invention using following principle, is directed to ingredient and content in waste liquor,
Sodium hydroxide solution is first added, in waste liquor beet alkali hydrochlorate and trimethylamine hydrochloride and hydrochloric acid carry out neutralization reaction,
Exothermic heat of reaction, part trimethylamine can escape in gaseous form, and the main component in waste liquor becomes water, glycine betaine, chlorination at this time
Sodium, hydroxy acid sodium, trimethylamine and other unknown materials.Then after waste liquor being concentrated, ethyl alcohol is added while hot, expects drop
To room temperature, filtering, since sodium chloride and hydroxy acid sodium do not dissolve in ethyl alcohol, the solubility of glycine betaine in ethanol is also than in water
In it is small, therefore, the main component of filter cake is sodium chloride, hydroxy acid sodium and glycine betaine, the main component in filtrate have ethyl alcohol,
Glycine betaine, sodium chloride, unknown material.Filter cake is recycled and generates added value, ethyl alcohol can recycling.
After using above-mentioned technical proposal, the beneficial effects of the invention are as follows：
Method provided by the invention is easy to operate, of low cost, and reaction is mild, low for equipment requirements, processed beet
Alkali sodium method synthesis technology waste liquor can be easily achieved separation of solid and liquid, the filter cake of the 55wt% of recyclable waste liquor amount, recycling
Filter cake can generate added value, the ethyl alcohol used in the process can be recycled by way of distillation, cost-effective, have it is larger
Economic value.
Specific implementation mode
With reference to specific embodiment, the present invention is further described.But the purposes and mesh of these exemplary embodiments
Be only used for enumerating the present invention, any type of any restriction not is constituted to the real protection scope of the present invention, it is more non-to incite somebody to action this
The protection domain of invention is confined to this.
Embodiment 1
The waste liquor for weighing the synthesis of 500g beet alkali hydrochlorate sodium methods is placed in more mouthfuls of 2L round-bottomed flasks, first presses 20ml/s
Rate be added, use the rate of 10ml/s later, first quick and back slow a concentration of 30% sodium hydroxide solution is added to pH=
7.5, the trimethylamine escaped is absorbed with water, and the consumption of 30% sodium hydroxide is 350g；
When temperature is down to 20 DEG C, the stirring concentration 2h under the conditions of 100 DEG C, vacuum degree 0.07MPa；
When temperature is down to 75 DEG C, absolute ethyl alcohol 100g is added while hot, during which stirs always on；
It when temperature is down to 20 DEG C, is filtered under the conditions of vacuum degree 0.07MPa, obtains filter cake 271g, filtrate 139g；
Filtrate is distilled, recycling ethyl alcohol 88g.
Filtrate component is analyzed：Glycine betaine, sodium chloride, ethyl alcohol, non-principal component, water.
Embodiment 2
The waste liquor of input 1000Kg beet alkali hydrochlorate sodium methods synthesis, the rate for first pressing 20ml/s are added in reaction kettle,
Use the sodium hydroxide solution of the addition a concentration of 30% of the rate of 5ml/s first quick and back slow to pH=7.0 later, three escaped
Methylamine is absorbed with water, and the consumption of 30% sodium hydroxide is 685Kg；
When temperature is down to 20 DEG C, lead to steam, the stirring concentration 1h under the conditions of 140 DEG C, vacuum degree 0.06MPa；
When temperature is down to 75 DEG C, absolute ethyl alcohol 50Kg is added while hot, during which stirs always on；
It when temperature is down to 20 DEG C, is filtered under the conditions of vacuum degree 0.06MPa, obtains filter cake 536Kg, filtrate 178Kg；
Filtrate is distilled, recycling ethyl alcohol 42kg.
Filtrate component is analyzed：Glycine betaine, sodium chloride, ethyl alcohol, non-principal component, water.
Embodiment 3
The method of the present embodiment includes the following steps：
(1) waste liquor is handled with a concentration of 30wt% sodium hydroxide solutions, and the rate for first pressing 20ml/s is added, Zhi Houyong
The rate of 5ml/s is added, and it is 7.0 that addition terminal, which is reaction solution pH, and the trimethylamine generated in the process is recycled with water；
(2) by step (1) reaction solution in 95 DEG C of temperature, pressure 0.07MPa is concentrated, and is concentrated into bubble-free and is produced as
Only；
(3) absolute ethyl alcohol is added while hot into concentrate obtained by step (2), amount of alcohol is the 5wt% of waste liquor amount, dense
Absolute ethyl alcohol is added when being 65 DEG C in contracting liquid, during which opens and stirs, stir speed (S.S.) 300rpm, when temperature is reduced to 20 DEG C,
Vacuum degree filters under the conditions of being 0.07MPa, and filter cake recycles；
(4) gained filtrate in step (3) is subjected to distillation processing, recycles ethyl alcohol.
Filtrate component is analyzed：Glycine betaine, sodium chloride, ethyl alcohol, non-principal component, water.
Embodiment 4
The method of the present embodiment includes the following steps：
(1) waste liquor is handled with a concentration of 30wt% sodium hydroxide solutions, and the rate for first pressing 25ml/s is added, Zhi Houyong
The rate of 10ml/s is added, and it is 8.0 that addition terminal, which is reaction solution pH, and the trimethylamine generated in the process is recycled with water；
(2) by step (1) reaction solution in 100 DEG C of temperature, pressure 0.07MPa is concentrated, and is concentrated into bubble-free and is produced as
Only；
(3) absolute ethyl alcohol is added while hot into concentrate obtained by step (2), amount of alcohol is the 25wt% of waste liquor amount, dense
Absolute ethyl alcohol is added when being 75 DEG C in contracting liquid, during which opens and stirs, stir speed (S.S.) 400rpm, when temperature is reduced to 25 DEG C,
Vacuum degree filters under the conditions of being 0.09MPa, and filter cake recycles；
(4) gained filtrate in step (3) is subjected to distillation processing, recycles ethyl alcohol.
Filtrate component is analyzed：Glycine betaine, sodium chloride, ethyl alcohol, non-principal component, water.
Embodiment 5
The method of the present embodiment includes the following steps：
(1) waste liquor is handled with a concentration of 30wt% sodium hydroxide solutions, and the rate for first pressing 22ml/s is added, Zhi Houyong
The rate of 8ml/s is added, and it is 7.5 that addition terminal, which is reaction solution pH, and the trimethylamine generated in the process is recycled with water；
(2) by step (1) reaction solution in 98 DEG C of temperature, pressure 0.07MPa is concentrated, and is concentrated into bubble-free and is produced as
Only；
(3) absolute ethyl alcohol is added while hot into concentrate obtained by step (2), amount of alcohol is the 15wt% of waste liquor amount, dense
Absolute ethyl alcohol is added when being 70 DEG C in contracting liquid, during which opens and stirs, stir speed (S.S.) 350rpm, when temperature is reduced to 24 DEG C,
Vacuum degree filters under the conditions of being 0.08MPa, and filter cake recycles；
(4) gained filtrate in step (3) is subjected to distillation processing, recycles ethyl alcohol.
Filtrate component is analyzed：Glycine betaine, sodium chloride, ethyl alcohol, non-principal component, water.
Comparative example 1
Using application No. is 201610629991.9, a kind of entitled beet alkali hydrochlorate calcium method production technology is useless female
The processing method of liquid in the waste liquor synthesized to beet alkali hydrochlorate sodium method, adds water to heat up, with sodium hydrate regulator solution pH,
It catches up with and removes alkaline gas, cooling is separated by solid-liquid separation, sulfuric acid is added in clear liquid, is separated by solid-liquid separation again, hydrochloric acid is added in clear liquid, is cooled down
Crystallization is separated by solid-liquid separation.
Filtrate component is analyzed：Beet alkali hydrochlorate, sodium chloride, hydrogen chloride, sulfuric acid, hydroxy acid sodium, sodium sulphate, it is unknown at
Divide, water.
Filtrate component is compared with embodiment 1-5：Hydrogen chloride, sodium chloride, sulfuric acid, sulfuric acid are newly introduced in comparative example 1
The impurity such as sodium increase the complexity of solution, increase intractability, and glycine betaine cannot recycle profit again from waste liquor
With；And a large amount of sodium chloride and hydroxy acid sodium may separate out using the present invention, contained only in solution after processing recycling ethyl alcohol glycine betaine,
A small amount of sodium chloride, ethyl alcohol, unknown material, water, greatly reduce complexity, while realizing that the glycine betaine in waste liquor effectively returns
It receives, there is larger economic implications.
It should be appreciated that the purposes of these embodiments is merely to illustrate the present invention and is not intended to limitation protection model of the invention
It encloses.In addition, it should also be understood that, after reading the technical contents of the present invention, those skilled in the art can make the present invention each
Kind change, modification and/or variation, all these equivalent forms equally fall within and are protected defined by the application the appended claims
Within the scope of shield.
Claims (9)
1. a kind of method of processing beet alkali hydrochlorate sodium method production technology waste liquor, it is characterised in that：Include the following steps：It will
Waste liquor first uses naoh treatment recovery section trimethylamine；Reaction solution is concentrated again, absolute ethyl alcohol is added while hot, is stirred to normal
It is filtered when warm, filtrate is distilled to recover ethyl alcohol.
2. a kind of method of processing beet alkali hydrochlorate sodium method production technology waste liquor as described in claim 1, feature exist
In：Include the following steps：
(1) waste liquor is handled with a concentration of 30wt% sodium hydroxide solutions, and the rate for first pressing 20-25ml/s is added, and uses 5- later
The rate of 10ml/s is added, and it is alkalescent that addition terminal, which is reaction solution pH, and the trimethylamine generated in the process is recycled；
(2) step (1) reaction solution is concentrated；
(3) absolute ethyl alcohol is added into concentrate obtained by step (2), filters, filter cake recycles；
(4) gained filtrate in step (3) is subjected to distillation processing, recycles ethyl alcohol.
3. a kind of method of processing beet alkali hydrochlorate sodium method production technology waste liquor as claimed in claim 2, feature exist
In：The trimethylamine generated in the process is recycled with water in step (1).
4. a kind of method of processing beet alkali hydrochlorate sodium method production technology waste liquor as claimed in claim 2, feature exist
In：It is 7.0-8.0 that waste liquor and the terminal of sodium hydroxide reaction, which are pH, in step (1).
5. a kind of method of processing beet alkali hydrochlorate sodium method production technology waste liquor as claimed in claim 2, feature exist
In：Reaction solution is in 95-100 DEG C of temperature, pressure 0.07MPa, until being concentrated into bubble-free generation in step (2).
6. a kind of method of processing beet alkali hydrochlorate sodium method production technology waste liquor as claimed in claim 2, feature exist
In：Absolute ethyl alcohol is added in step (3) while hot, and stirs, amount of alcohol is 5wt% -25wt% of waste liquor amount.
7. a kind of method of processing beet alkali hydrochlorate sodium method production technology waste liquor as claimed in claim 2, feature exist
In：Absolute ethyl alcohol is added when concentrate is 65-75 DEG C in step (3), during which opens stirring, stir speed (S.S.) 300-
400rpm。
8. a kind of method of processing beet alkali hydrochlorate sodium method production technology waste liquor as claimed in claim 2, feature exist
In：In step (3) when temperature is reduced to 20-25 DEG C, filtered under the conditions of vacuum degree is 0.07-0.09MPa.
9. such as a kind of method of processing beet alkali hydrochlorate sodium method production technology waste liquor of claim 1-8 any one of them,
It is characterized in that：Steps are as follows：
The waste liquor for weighing the synthesis of beet alkali hydrochlorate sodium method is placed in more mouthfuls of round-bottomed flasks, and the rate for first pressing 20ml/s is added,
The sodium hydroxide solution of a concentration of 30wt% is added to pH=7.5 with the rate of 5ml/s later, the trimethylamine escaped is inhaled with water
It receives；
It is 100 DEG C to be heated to temperature, and under the conditions of vacuum degree 0.07MPa, stir speed (S.S.) is 400rpm stirring concentration 2h, is concentrated into nothing
Until bubble generates；
When temperature is down to 75 DEG C, absolute ethyl alcohol is added while hot, during which always on stirring, rate 400rpm；
When temperature is down to 20 DEG C, is filtered under the conditions of vacuum degree 0.07MPa, obtain filter cake, filtrate；
Filtrate is distilled, ethyl alcohol is recycled.
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| CN201810378870.0A CN108440321A (en) | 2018-04-25 | 2018-04-25 | A method of processing beet alkali hydrochlorate sodium method production technology waste liquor |
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| CN201810378870.0A CN108440321A (en) | 2018-04-25 | 2018-04-25 | A method of processing beet alkali hydrochlorate sodium method production technology waste liquor |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1844082A (en) * | 2006-04-26 | 2006-10-11 | 潍坊祥维斯化学品有限公司 | Process for preparing betaine |
| CN101863784A (en) * | 2010-06-07 | 2010-10-20 | 房照智 | Methods for preparing and extracting betaine and betaine hydrochloride |
| 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 |
| CN104054912A (en) * | 2014-06-11 | 2014-09-24 | 山东奥克特化工有限公司 | Method for producing betaine powder by residual mother solution in process of extracting betaine hydrochloride |
| CN106220520A (en) * | 2016-08-04 | 2016-12-14 | 山东省化工研究院 | A kind of processing method of beet alkali hydrochlorate calcium method production technology waste liquor |
-
2018
- 2018-04-25 CN CN201810378870.0A patent/CN108440321A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1844082A (en) * | 2006-04-26 | 2006-10-11 | 潍坊祥维斯化学品有限公司 | Process for preparing betaine |
| CN101863784A (en) * | 2010-06-07 | 2010-10-20 | 房照智 | Methods for preparing and extracting betaine and betaine hydrochloride |
| 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 |
| CN104054912A (en) * | 2014-06-11 | 2014-09-24 | 山东奥克特化工有限公司 | Method for producing betaine powder by residual mother solution in process of extracting betaine hydrochloride |
| CN106220520A (en) * | 2016-08-04 | 2016-12-14 | 山东省化工研究院 | A kind of processing method of beet alkali hydrochlorate calcium method production technology waste liquor |
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| 郝立勇 等: "化学法合成甜菜碱工艺的改进", 《中国甜菜糖业》 * |
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Application publication date: 20180824 |