CN107868241A - A kind of fatty alcohol block polyether class tar ammonia demulsifier and preparation method thereof - Google Patents
A kind of fatty alcohol block polyether class tar ammonia demulsifier and preparation method thereof Download PDFInfo
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- CN107868241A CN107868241A CN201711186447.2A CN201711186447A CN107868241A CN 107868241 A CN107868241 A CN 107868241A CN 201711186447 A CN201711186447 A CN 201711186447A CN 107868241 A CN107868241 A CN 107868241A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/26—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds
- C08G65/2603—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen
- C08G65/2606—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen containing hydroxyl groups
- C08G65/2609—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen containing hydroxyl groups containing aliphatic hydroxyl groups
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G33/00—Dewatering or demulsification of hydrocarbon oils
- C10G33/04—Dewatering or demulsification of hydrocarbon oils with chemical means
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Abstract
The present invention proposes a kind of efficiently polymer electrolyte fat alcohol block polyether class tar ammonia demulsifier and preparation method thereof, belong to coking of coal technical field, the polymer electrolyte fat alcohol block polyether class compound being prepared by the preparation method, it is low with chemical feeding quantity, quickly break Water-In-Oil, oil-in-water system, destroy the effect that oil-water emulsion layer promotes water-oil separating, having concurrently simultaneously reduces cyclic ammonia water oil content, distilled ammonia wastewater COD is reduced, shortens the dehydration of tar time, reduces the significant advantages such as energy consumption.The technical scheme is included to substitute multi-alcohol as initiator, and it using polyalkylene oxide A is a kind of polymeric fatty alcohol block polyether class demulsifier of the hydrophobic grouping using polycyclic alkane B as hydrophilic radical to be copolymerized obtained by epoxyalkane A, epoxyalkane B block.The present invention can be applied to coke-oven plant's tar ammonia demulsification field.
Description
Technical field
The invention belongs to coking of coal industry tar ammonia break milk separation technical field, more particularly to a kind of polymer electrolyte fat
Alcohol block polyether class tar ammonia demulsifier and preparation method thereof.
Background technology
In coking of coal industry process of coking, coking by coke oven coal gas needs to condense by ammonia spray, and condensate liquid contains largely
Tar, tar slag, the material such as ammoniacal liquor containing quinoline insolubles.Mechanical defecator is primarily used to separate ammoniacal liquor, tar and Jiao
The dregs of fat, influenceed due to carrying coal dust and organic matter in by residence time, coke-stove gas secretly, mechanical defecator separating effect can be big
Give a discount, cause tar water content exceeded when serious, make the reduction of tar price, cause cyclic ammonia water, remained ammonia oil content to increase
It is more, the reuse of cyclic ammonia water is influenceed, while the COD for also influenceing follow-up distilled ammonia wastewater is removed, and increases the environmentally friendly cost of enterprise.
At present, the mode of natural subsidence is generally taken to carry out tar ammonia separation, but sedimentation time length be present in this method, point
Poor from effect, tar is aqueous easily exceeded, the shortcomings of ammoniacal liquor oil content is high, a kind of efficiently polymer electrolyte fat involved in the present invention
Alcohol block polyether uses as tar ammonia demulsifier can quickly break Water-In-Oil, oil-in-water system, promote water-oil separating.
The A of patent CN 102432741, one kind are disclosed with methanol, toluene dimethylbenzene is the tar ammonia demulsifier of solvent
Preparation method, wherein, organic high molecular polymer is dissolved in methanol, tar ammonia demulsifier is used as in toluene or dimethylbenzene,
Successfully shorten the water-oil separating time.
However, in the above-mentioned methods, by the way of the organic solvent based composition such as high molecular polymer and methanol toluene
Tar ammonia water mixture is demulsified, this there is, and demulsifier toxicity is big and flash-point is low, inflammable and explosive, should not transport storage,
And a large amount of a series of problems, such as polluting and its being unfavorable for health and safety green production are produced during production or use to environment.
The content of the invention
The invention provides a kind of efficiently polymer electrolyte fat alcohol block polyether class tar ammonia demulsifier and its preparation side
Method, the molecule-type fat alcohol block polyether being prepared by the preparation method can be used as tar ammonia demulsifier, have chemical feeding quantity
It is low, quickly break Water-In-Oil, oil-in-water system, destroy oil-water emulsion layer and promote the effect of water-oil separating, while have reduction concurrently and follow
Ring ammoniacal liquor oil content, distilled ammonia wastewater COD is reduced, shorten the dehydration of tar time, reduce the significant advantages such as energy consumption.
In order to achieve the above object, an aspect of of the present present invention provides a kind of preparation of polymer electrolyte fat alcohol block polyether
Method, comprise the following steps：
Using substituting multi-alcohol that polyaddition reaction occurs under acidic catalyst effect for initiator and epoxyalkane A,
Obtain a kind of aliphatic alcohol polyether；
Open loop sudden reaction occurs under base catalyst effect using the aliphatic alcohol polyether and epoxyalkane B, obtains target
Product fatty alcohol block polyether.
As optimal technical scheme, the polyaddition reaction is specially：
The substitution multi-alcohol is with epoxyalkane A with mol ratio 1:100-500 makees in aromatic solvent in acidic catalyst
Under, in 90 DEG C -150 DEG C in nitrogen atmosphere, sudden reaction 3-6 hours occur, obtain a kind of aliphatic alcohol polyether.
As optimal technical scheme, the open loop sudden reaction is specially：
The aliphatic alcohol polyether, in nitrogen atmosphere at a temperature of 120 DEG C -150 DEG C, under base catalyst effect, with epoxy
Alkane B reacts 2-6 hours；The epoxyalkane B and the mol ratio of aliphatic alcohol polyether wherein added is 1:5-16.
As optimal technical scheme, the contraposition that the substitution multi-alcohol is selected from C2-C22 straight or branched alkane substitutes
Alcohol.
As optimal technical scheme, the epoxyalkane A be expoxy propane, chloro- 2, the 3- expoxy propane of 1-, 1,2- epoxies-
One or more in 3- methybutanes, 2- methoxyl group epoxy butanes.
As optimal technical scheme, the epoxyalkane B is selected from least one of oxirane or methyl oxirane.
As optimal technical scheme, the acidic catalyst in acetic acid, concentrated hydrochloric acid or p-methyl benzenesulfonic acid at least one
Kind, the base catalyst in tungsten oxide-zirconium oxide, molybdenum oxide-zirconium oxide, potassium hydroxide or sodium hydroxide at least one
Kind.
Another aspect of the present invention additionally provides the fatty alcohol block polyether described in a kind of technical scheme of any one as described above
The preparation-obtained fatty alcohol block polyether of preparation method, it is characterised in that there is following structural formula：
Wherein, n=1-4；x=5-16；y=100-500；R is C2-C22 straight or branched alkyls；R ' is methyl or contains methoxy
The direct-connected or branched alkane alkyl of base or halogenic substituent.
Another aspect of the invention additionally provides a kind of fatty alcohol block polyether as described in above-mentioned technical scheme by certain
Application of the aqueous solution as tar ammonia demulsifier in coke-oven plant's tar ammonia fast emulsion breaking separation field after dilution proportion.
Compared with prior art, advantage possessed by the present invention and beneficial effect are：
1st, the preparation-obtained fatty alcohol block polyether of preparation method provided by the present invention, it is water soluble oil parting polymer, makees
Need to only to be compounded by a certain percentage with water during tar ammonia demulsifier use, without being compounded with organic solvents such as methanol toluenes, i.e.,
It can play a part of accelerating water-oil separating to promote demulsification, and with chemical feeding quantity is low, rapid damage oil-water emulsion layer promotes profit
The effect of separation, while have reduction cyclic ammonia water oil content concurrently, distilled ammonia wastewater COD is reduced, shortens the dehydration of tar time, reduces energy
The significant advantages such as consumption, are a kind of efficient and environment-friendly type tar ammonia demulsifiers.
2nd, the preparation-obtained fatty alcohol block polyether of preparation method provided by the present invention using water as solvent complex and
Into tar ammonia demulsifier compared with the tradition demulsifier that organic molten compounding forms with methanol or toluene dimethylbenzene etc., there is life
Produce and small using process environmental protection, pollution；Flash-point is high, is easy to transport storage；It is nontoxic, reduce the health hazard to operating personnel
Etc. advantage.
3rd, the raw material sources selected by preparation method provided by the present invention are extensive, and production cost is low, and reaction condition is gentle,
It is easy to industrialization continuity production.
Embodiment
The technical scheme in the embodiment of the present invention will be clearly and completely described below, it is clear that described embodiment is only
Only it is part of the embodiment of the present invention, rather than whole embodiments.Based on the embodiment in the present invention, ordinary skill
The every other embodiment that personnel are obtained under the premise of creative work is not made, belongs to the scope of protection of the invention.
The one side of the embodiment of the present invention provides a kind of preparation method of fatty alcohol block polyether, comprises the following steps：
S1：It is anti-using substituting multi-alcohol that addition polymerization occurs under acidic catalyst effect for initiator with epoxyalkane A
Should, obtain a kind of aliphatic alcohol polyether；
S2：Open loop sudden reaction occurs under base catalyst effect using the aliphatic alcohol polyether and epoxyalkane B, obtains mesh
Mark product fatty alcohol block polyether.
In the above embodiment of the present invention, directly urged using substitution multi-alcohol with epoxyalkane A and epoxyalkane B
Target product can obtain by differential responses step in the presence of agent.Using the target product obtained by the preparation method-
After fatty alcohol block polyether and water compound, you can play a part of accelerating the demulsification layering of tar ammonia mixture, and have and add
Dose is low, rapid damage oil-water emulsion layer promotes the effect of water-oil separating, while has reduction cyclic ammonia water oil content concurrently, reduces and steams
Ammonia waste water COD, shorten the dehydration of tar time, reduce the significant advantages such as energy consumption, be a kind of efficient and environment-friendly type tar ammonia demulsifier,
Quality assurance is provided for coking production and tar following process.
Only it is that to list a kind of reaction condition gentle, efficiency high, suitable for large-scale production in the present embodiment
Synthesis mode, can be not limited to cited mode, and those skilled in the art can also select to close according to actual production conditions
Reason, the other manner of optimization are replaced, as long as can obtain being expected product.
To make the purpose, technical scheme and advantage of the embodiment of the present invention clearer, below in conjunction with the embodiment of the present invention.
Clear, complete description is carried out to the technical scheme in the embodiment of the present invention, it is clear that described embodiment is the present invention one
Divide embodiment, rather than whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art are not making
The every other embodiment obtained on the premise of inventive improvements, belong to the category that the present invention protects.
Embodiment 1：
In 2 cubic metres of stainless steel cauldrons, it is 1 part to add the initiator mol ratio containing catalyst prepared in advance
Substitute fatty alcohol, first with the air in nitrogen displacement reactor, then be warming up to 100 DEG C, start to open initiator circulating pump,
Initiator adds the epoxyalkane A that mol ratio is 100 parts, the speed of addition is using energy keeping temperature as 100 DEG C under spray form
Be advisable, and control reaction pressure, until finishing, and slaking reaction gone down after a rise to pressure after add epoxyalkane B, add speed
Depending on temperature, pressure and adjust, after mol ratio is that 15 parts of epoxyalkane B is finished, then slaking reaction to pressure is gone down after a rise, and is cooled to
It is 7 that 90 DEG C of addition glacial acetic acid, which are neutralized to pH, and the salt for neutralizing generation adds filter aid to be removed while hot with mechanical filter, and filtrate is institute
The fatty alcohol block polyether needed.
Embodiment 2:
In 2 cubic metres of stainless steel cauldrons, it is 1 part to add the initiator mol ratio containing catalyst prepared in advance
Substitute fatty alcohol, first with the air in nitrogen displacement reactor, then be warming up to 120 DEG C, start to open initiator circulating pump,
Initiator adds the epoxyalkane A that mol ratio is 100 parts, the speed of addition is using energy keeping temperature as 120 DEG C under spray form
Be advisable, and control reaction pressure, until finishing, and slaking reaction gone down after a rise to pressure after add epoxyalkane B, add speed
Depending on temperature, pressure and adjust, after mol ratio is that 15 parts of epoxyalkane B is finished, then slaking reaction to pressure is gone down after a rise, and is cooled to
It is 7 that 90 DEG C of addition glacial acetic acid, which are neutralized to pH, and the salt for neutralizing generation adds filter aid to be removed while hot with mechanical filter, and filtrate is institute
The fatty alcohol block polyether needed.
Embodiment 3:
In 2 cubic metres of stainless steel cauldrons, it is 1 part to add the initiator mol ratio containing catalyst prepared in advance
Substitute fatty alcohol, first with the air in nitrogen displacement reactor, then be warming up to 140 DEG C, start to open initiator circulating pump,
Initiator adds the epoxyalkane A that mol ratio is 100 parts, the speed of addition is using energy keeping temperature as 140 DEG C under spray form
Be advisable, and control reaction pressure, until finishing, and slaking reaction gone down after a rise to pressure after add epoxyalkane B, add speed
Depending on temperature, pressure and adjust, after mol ratio is that 15 parts of epoxyalkane B is finished, then slaking reaction to pressure is gone down after a rise, and is cooled to
It is 7 that 90 DEG C of addition glacial acetic acid, which are neutralized to pH, and the salt for neutralizing generation adds filter aid to be removed while hot with mechanical filter, and filtrate is institute
The fatty alcohol block polyether needed.
Embodiment 4:
In 2 cubic metres of stainless steel cauldrons, it is 1 part to add the initiator mol ratio containing catalyst prepared in advance
Substitute fatty alcohol, first with the air in nitrogen displacement reactor, then be warming up to 140 DEG C, start to open initiator circulating pump,
Initiator adds the epoxyalkane B that mol ratio is 15 parts under spray form, and the speed of addition is as 140 DEG C using energy keeping temperature
Preferably, and control reaction pressure, until finishing, and slaking reaction gone down after a rise to pressure after add epoxyalkane A, add speed and regard
Temperature, pressure and adjust, after mol ratio is that 100 parts of epoxyalkane A is finished, then slaking reaction to pressure is gone down after a rise, and is cooled to
It is 7 that 90 DEG C of addition glacial acetic acid, which are neutralized to pH, and the salt for neutralizing generation adds filter aid to be removed while hot with mechanical filter, and filtrate is institute
The fatty alcohol block polyether needed.
Embodiment 5:
In 2 cubic metres of stainless steel cauldrons, it is 1 part to add the initiator mol ratio containing catalyst prepared in advance
Substitute fatty alcohol, first with the air in nitrogen displacement reactor, then be warming up to 140 DEG C, start to open initiator circulating pump,
Initiator adds the epoxyalkane B that mol ratio is 10 parts under spray form, and the speed of addition is as 140 DEG C using energy keeping temperature
Preferably, and control reaction pressure, until finishing, and slaking reaction gone down after a rise to pressure after add epoxyalkane A, add speed and regard
Temperature, pressure and adjust, after mol ratio is that 500 parts of epoxyalkane A is finished, then slaking reaction to pressure is gone down after a rise, and is cooled to
It is 7 that 90 DEG C of addition glacial acetic acid, which are neutralized to pH, and the salt for neutralizing generation adds filter aid to be removed while hot with mechanical filter, and filtrate is institute
The fatty alcohol block polyether needed.
Performance test：
Shandong coke-oven plant is circulated after being compounded by a certain percentage using the fatty alcohol block polyether obtained by embodiment 1-5 and water
Ammoniacal liquor water sample carries out the de-oiling measure of merit that is demulsified, and experiment process is as follows：65-75 DEG C will be preheated in cyclic ammonia water water sample water-bath
Afterwards, 6 parts of water samples are taken respectively, and every part of 250ml is placed in 500ml separatory funnels, stays a blank, and other are respectively to separatory funnel
Add 20ppm embodiment 1-5 synthesis fatty alcohol block polyether, at the uniform velocity stir 3 minutes, stand half an hour, after take mid-water
Sample, using national standard gravimetric detemination oil content, to determine oil-water separation.
The polymer demulsification performance comparing result of 1. different embodiments of table synthesis
As can be seen from Table 1, the fatty alcohol block polyether that the embodiment of the present invention is provided promotes what is be demulsified to having containing tar ammonia
Effect, preferably demulsification de-oiling effect is can reach in standing 30min or so after dosing,.In addition, surveyed through same experiment process
Fixed, the polymer demulsification synthesized prepared by the embodiment of the present invention 3 is ideal.
Demulsification contrasts
Choose domestic Jinan, Shandong Province company tar ammonia demulsifier agent A, company of the demulsifier B U.S. of company of Langfang in Hebei Province G
Tar ammonia demulsifier C and company of U.S. N tar ammonia agent D enter with the tar ammonia demulsifier obtained by embodiment 3
Row check experiment, dosing dosage 20ppm, experiment process are same as above, and the results are shown in Table 2：
Table 2:Different sedimentation agent performance comparisons
By experimental result as can be seen that made products have been issued to the demulsification of imported product in identical dosing dosage.
Claims (9)
- A kind of 1. preparation method of efficiently polymer electrolyte fat alcohol block polyether class tar ammonia demulsifier, it is characterised in that bag Include following steps：Using substituting multi-alcohol that polyaddition reaction occurs under acidic catalyst effect for initiator and epoxyalkane A, Obtain a kind of aliphatic alcohol polyether；Open loop sudden reaction occurs under base catalyst effect using the aliphatic alcohol polyether and epoxyalkane B, obtains target Product fatty alcohol block polyether.
- 2. preparation method according to claim 1, it is characterised in that the polyaddition reaction is specially：The substitution multi-alcohol is with epoxyalkane A with mol ratio 1:100-500 makees in aromatic solvent in acidic catalyst Under, in 90 DEG C -150 DEG C in nitrogen atmosphere, sudden reaction 3-6 hours occur, obtain a kind of aliphatic alcohol polyether.
- 3. preparation method according to claim 1, it is characterised in that the open loop sudden reaction is specially：The aliphatic alcohol polyether, in nitrogen atmosphere at a temperature of 120 DEG C -150 DEG C, under base catalyst effect, with epoxy Alkane B reacts 2-6 hours；The epoxyalkane B and the mol ratio of aliphatic alcohol polyether wherein added is 1:5-16.
- 4. preparation method according to claim 1 or 2, it is characterised in that the substitution multi-alcohol is selected from C2-C22 The contraposition substituted alcohols of straight or branched alkane.
- 5. preparation method according to claim 1 or 2, it is characterised in that the epoxyalkane A is expoxy propane, 1- is chloro- One or more in 2,3- expoxy propane, 1,2- epoxy -3- methybutanes, 2- methoxyl group epoxy butanes.
- 6. the preparation method according to claim 1 or 3, it is characterised in that the epoxyalkane B is selected from oxirane or first At least one of hexadecyl ethylene oxide.
- 7. preparation method according to claim 1, it is characterised in that the acidic catalyst be selected from acetic acid, concentrated hydrochloric acid or At least one of p-methyl benzenesulfonic acid, the base catalyst are selected from tungsten oxide-zirconium oxide, molybdenum oxide-zirconium oxide, potassium hydroxide Or at least one of sodium hydroxide.
- A kind of 8. preparation-obtained fatty alcohol of preparation method of fatty alcohol block polyether as described in claim any one of 1-7 Block polyether, it is characterised in that there is following structural formula：Wherein, n=1-4；x=5-16；y=100-500；R is C2-C22 straight or branched alkyls；R ' is methyl or contains methoxy The direct-connected or branched alkane alkyl of base or halogenic substituent.
- 9. a kind of fatty alcohol block polyether as claimed in claim 8 dilute by a certain percentage after the aqueous solution as tar ammonia Application of the demulsifier in coke-oven plant's tar ammonia fast emulsion breaking separation field.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109517160A (en) * | 2018-11-28 | 2019-03-26 | 宁波润禾高新材料科技股份有限公司 | A kind of preparation method of secondary amine type polyetheramine |
| CN110408017A (en) * | 2019-07-15 | 2019-11-05 | 佳化化学科技发展（上海）有限公司 | It is a kind of fat alcohol block polyether, for dispersing agent of pesticide suspension concentrate and preparation method thereof, pesticide suspension concentrate |
| CN113072695A (en) * | 2021-03-30 | 2021-07-06 | 浙江皇马科技股份有限公司 | Preparation method of foam stabilizing surfactant with good low-temperature fluidity |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109517160A (en) * | 2018-11-28 | 2019-03-26 | 宁波润禾高新材料科技股份有限公司 | A kind of preparation method of secondary amine type polyetheramine |
| CN110408017A (en) * | 2019-07-15 | 2019-11-05 | 佳化化学科技发展（上海）有限公司 | It is a kind of fat alcohol block polyether, for dispersing agent of pesticide suspension concentrate and preparation method thereof, pesticide suspension concentrate |
| CN110408017B (en) * | 2019-07-15 | 2022-03-22 | 佳化化学科技发展（上海）有限公司 | Fatty alcohol block polyether, dispersing agent for pesticide aqueous suspension agent, preparation method of dispersing agent and pesticide aqueous suspension agent |
| CN113072695A (en) * | 2021-03-30 | 2021-07-06 | 浙江皇马科技股份有限公司 | Preparation method of foam stabilizing surfactant with good low-temperature fluidity |
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Application publication date: 20180403 |