CN108003909A - A kind of composite demulsifying agent for wood tar dehydration - Google Patents
A kind of composite demulsifying agent for wood tar dehydration Download PDFInfo
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- CN108003909A CN108003909A CN201810002081.7A CN201810002081A CN108003909A CN 108003909 A CN108003909 A CN 108003909A CN 201810002081 A CN201810002081 A CN 201810002081A CN 108003909 A CN108003909 A CN 108003909A
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- Prior art keywords
- composite demulsifying
- demulsifier
- wood tar
- initiator
- agent
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C1/00—Working-up tar
- C10C1/02—Removal of water
Abstract
The present invention relates to biomass energy technology field, and in particular to a kind of dehydration technique suitable for biomass pyrolytic charing product.The present invention have developed new composite demulsifying agent for wood tar first, can be suitable for the dehydration of wood tar.It can play the role of solubilising by adding auxiliary agent, is scattered with adjusting pH value, without adding other acid-base modifiers again, and by the synergistic effect between polyether type demulsifying agent and fluorocarbon surfactant and auxiliary agent, reaching the effect of breaking emulsion and dewatering.Composite demulsifying agent provided by the invention, it is good to can be applied to wood tar, broad spectrum activity obtained by a variety of biomass carbonated pyrolysis, and interface is clear after being demulsified, demulsification is good, and the wood tar water content after dehydration is low.Reagent is known or available material used by compounding, has saved the cost needed for a large amount of synthesis new products, has realized the production of demulsifier high efficiency, low cost.
Description
Technical field
The present invention relates to biomass energy technology field, and in particular to a kind of dehydration technique of biomass pyrolytic charing product.
Background technology
Biomass pyrolytic charing technology is a kind of biomass energy utilization technology for having very much development prospect.By to biology
Matter, which carries out pyrolysis charring, can obtain gas, the thermal decomposition product of solid two class kenels, wherein, it is biomass carbon after solid product cooling；
And purified again, separation can then obtain biological fuel gas, wood tar and wood vinegar after gaseous products cooling.
Wherein, wood tar for using hydro carbons, acids and phenols as main component black, thick mixing liquid, by into
One step, which is processed wood tar, can obtain the products such as biomass fuel, creasote, wood pitch.However, also contain in wood tar
There are substantial amounts of moisture and solid impurity, this can not only damage follow-up process equipment, can also increase the energy consumption of processing, because
This, it is necessary to remove solid impurity and moisture therein before to wood tar working process；Wherein, solid impurity includes toluene
The larger solia particle such as the polymer particles such as the condensation polymer of insoluble matter, ash content and powdered carbon.For this fraction solids impurity
Processing, typically removes most of powdered carbon, ash grades solid impurity first with the mode of sedimentation, then is filtered further to remove
Remove remaining solid impurity.
And for the removing of moisture in wood tar, the mode of sedimentation is also only through at present to realize.But wood tar is
One kind typically further includes liquid phase particulate compared with thick liquid dispersion, its dispersed phase in addition to including solid impurity, is specially water
Particulate and various salting liquid particulates are dripped, these particulates, which are dispersed in oil medium, forms homogeneous system -- emulsion, and also wood is burnt
The presence of the compound such as phenol, aldehyde, ketone, carboxylic acid in oil, and the water phase in wood tar emulsion is reduced with oil phase density contrast, so
The emulsion quite stable of formation, when this allows for being dehydrated wood tar using subsidence style, speed is very slow, limited
Time in can not realize the complete dehydration of wood tar, this not only extends the overall production cycle of wood tar product, wood tar
In the moisture that does not remove can also bring harmful effect to subsequent technique.It is therefore desirable to effective dehydration is carried out to wood tar.
In the prior art, wood tar is not belonging to crude oil and petroleum product category, presently disclosed both for crude oil or stone
The demulsification processing of oil product, such as Chinese patent literature CN201693846 disclose one kind and are suitable for oil field and oil plant electricity
The demulsifier of desalination, its by 36%~50% polyethers demulsifier, 5%~10% fluorocarbon surfactant and 40%~
59% solvent composition.But the demulsifier is to be directed to oil field and desalting in oil refinery and research and develop obtained, is not particularly suited for wood
The dehydration of tar, uses it for that preferable demulsification can not be played in wood tar.
The content of the invention
The technical problems to be solved by the invention are to overcome demulsifier of the prior art can not reach preferable to wood tar
The defects of demulsification, and then a kind of demulsifier suitable for wood tar dehydration is provided, to realize wood tar is quick, high-quality dehydration.
The present invention realizes above-mentioned purpose by using following technical solution：
A kind of composite demulsifying agent, by weight, its composition include：
20~50 parts of polyethers demulsifier, 1~5 part of auxiliary agent, 2~5 parts of fluorocarbon surfactant, 35~60 parts of solvent.
The composite demulsifying agent, by weight, its composition include：40~50 parts of polyethers demulsifier, auxiliary agent 2~3
Part, 3~5 parts of fluorocarbon surfactant, 40~50 parts of solvent.
Also contain anion surfactant, cationic surfactant or both sexes class surface in the polyethers demulsifier
One or more in activating agent.
The polyethers demulsifier includes the block polyether using amine as initiator.
The polyethers demulsifier includes the block polyether using amine and alcohols as initiator respectively.
By weight, the ratio respectively using amine and alcohols as the block polyether of initiator is 5:4~4:5.
The polyethers demulsifier includes the block polyether using amine and alkyl phenolic resin as initiator respectively.
By weight, the ratio respectively using amine and alkyl phenolic resin as the block polyether of initiator is 5:4
~4:5.
The polyethers demulsifier includes DP classes demulsifier and the block polyether using alcohols as initiator.
By weight, the DP classes demulsifier and the ratio using alcohols as the block polyether of initiator are 5:4~4:5.
Wherein, the DP classes demulsifier is purchased from Jingzhou City of Hubei Province day and closes scientific and technological Chemical Co., Ltd..
The auxiliary agent has been reagent that is solubilized, scattered or adjusting one or two kinds of effects in pH value
The auxiliary agent is the one or more in organic acid, inorganic acid, short-chain branch alcohol or alcohol ether.
The organic acid is alkyl benzene sulphonate, acetic acid, oxalic acid, butanedioic acid, tartaric acid, benzoic acid, caffeic acid or salicylic acid
In one or more, the short-chain branch alcohol is butanol, the mixture of isopropanol or both, and the alcohol ether is isopropyl ether or second two
Alcohol ether.
The fluorocarbon surfactant is the surfactant obtained by the fluorine atom all hydrogen atom on substitution hydrocarbon chain.
The fluorocarbon surfactant is perfluorinated nonene base benzene sulfonic acid sodium salt, Sodium perfluorooctanoate or perfluoro-ethyl diethanol amine phosphorus
One or more in sour sodium.
The solvent is the one or more in oil-dissolving solvent, including solvent naphtha, aromatic solvent, oil-soluble alcohol.
The solvent is the one or more in water-soluble solvent, including water, water-soluble alcohol.
The composite demulsifying agent is used for realizing the purposes of wood tar dehydration.
The dosage of the composite demulsifying agent is 5~20ppm, and the temperature for the operation that is demulsified is 50~120 DEG C.
The purposes, includes the following steps：
Wood tar raw material is filtered, collects filtrate；
The filtrate is mixed with the demulsifier, obtains mixed liquor；
The mixed liquor is settled, water phase is then removed, that is, obtains dewatered wood tar.
The purposes further includes the step of being diluted to the wood tar raw material, and the wood tar after dilution carried out again
Filter and subsequent step.
It is provided by the invention to be had the following advantages suitable for the composite demulsifying agent of wood tar dehydration and its application：
1. the present invention have developed new composite demulsifying agent for wood tar first, the de- of wood tar can be suitable for
Water.The auxiliary agent that is added of the present invention can play the role of solubilising, is scattered with adjusting pH value, without adding other acid-base accommodations again
Agent, and pass through the synergistic effect between polyether type demulsifying agent and fluorocarbon surfactant and auxiliary agent so that demulsifier dissolubility
Strengthen and can quick adsorption in wood tar lotion oil with the interfacial film between water phase microlayer model, effectively reduce interface open
Power, makes moisture film and oil film gradually thinning, so as to reduce the boundary strength of moisture film and oil film, ultimately results in interfacial film rupture so that
With the polymerization of fluid drops of phase, reach the effect of breaking emulsion and dewatering.
Composite demulsifying agent provided by the invention, it is good to can be applied to wood tar, broad spectrum activity obtained by a variety of biomass carbonated pyrolysis,
And interface is clear after being demulsified, demulsification is good, and the wood tar water content after dehydration is low.Reagent is used by compounding
Known or available material, has saved the cost needed for a large amount of synthesis new products, has realized the production of demulsifier high efficiency, low cost.
2. composite demulsifying agent provided by the invention, by the further preferred of each component and content, using various poly-
Synergistic effect between ethers demulsifier, can accelerate the speed that demulsifier is adsorbed in oil/water interface, improve phase separation, make
Obtain wood tar and can reach preferable dehydrating effect in 15 minutes, greatly improve the pre-treating speed and quality of wood tar,
Shorten the production cycle that high level product is further obtained using wood tar.
3. the dehydration of wood tar is carried out using composite demulsifying agent provided by the present invention, loose operation condition,
It is operable within the temperature range of 50 DEG C~120 DEG C, and the demulsifier dosage of 5~20ppm is only needed, it is extremely low with regard to water content can be obtained
Wood tar, can effectively reduce the moisture infringement to equipment and the consumption to the energy in subsequent processing in wood tar, drop
The production cost of low wood tar depths products.
Embodiment
Technical scheme will be clearly and completely described below, it is clear that described embodiment is this hair
Bright part of the embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not having
All other embodiments obtained under the premise of creative work are made, belong to the scope of protection of the invention.In addition, following institute
As long as involved technical characteristic does not form conflict and be combined with each other each other in the different embodiments of the present invention of description.
The composite demulsifying agent that following embodiments are provided, by the way that each component uniform dissolution can obtain in solvent.
Polyethers demulsifier is commercially available finished product reagent used by following embodiments, it is of course also possible to use homemade polyethers are broken
Emulsion prepares composite demulsifying agent provided by the present invention.
Embodiment 1
Oil-soluble composite demulsifying agent provided in this embodiment for wood tar dehydration, consisting of：Using amine as starting
The block polyether class demulsifier AP221 45g of agent, Sodium perfluorooctanoate 5g, dodecyl benzene sulfonic acid and isopropanol mixture 3g, weight
Aromatic solvent 1000# 47g。
Embodiment 2
Oil-soluble composite demulsifying agent provided in this embodiment for wood tar dehydration, consisting of：With alkyl phenolic
Resin is the block polyether class demulsifier AR36 23g, the block polyether class demulsifier AE8051 using amine as initiator of initiator
20g, perfluorinated nonene epoxide benzene sulfonic acid sodium salt 3g, dodecyl benzene sulfonic acid and isopropanol mixture 4g, aromatic solvent 150# 50g。
Embodiment 3
Water Soluble Compound type demulsifier provided in this embodiment for wood tar dehydration, consisting of：Using amine as starting
The block polyether class demulsifier AE8051 20g of agent, the block polyether class demulsifier BP2040 25g using alcohol as initiator, perfluor
The methanol aqueous solution 48g of the mixture 2g, 20wt% of Sodium Caprylate 3g, acetic acid and butanol.
Embodiment 4
Water Soluble Compound type demulsifier provided in this embodiment for wood tar dehydration, consisting of：Polyethers are demulsified
Agent DP05 25g, block polyether class de-emulsifier SP 04 25g using alcohol as initiator, Sodium perfluorooctanoate 4g, acetic acid and butanol it is mixed
Compound 2g, methanol and ethanol mixed aqueous solution 44g, quality compare methanol：Ethanol：Water=1:2:1.
Wherein, DP05 and SP04 is purchased from Jingzhou City of Hubei Province day and closes scientific and technological Chemical Co., Ltd..
Embodiment 5
Oil-soluble composite demulsifying agent provided in this embodiment for wood tar dehydration, consisting of：With alkyl phenolic
Resin is the block polyether class demulsifier AR36 20g, the block polyether class demulsifier AE8051 using amine as initiator of initiator
21g, methyl hexadecanoate sodium sulfonate 3g, perfluoro-ethyl diethanol amine sodium phosphate 4g, ethylene glycol ethyl ether 2g, water 50g.
Embodiment 6
Water Soluble Compound type demulsifier provided in this embodiment for wood tar dehydration, consisting of：Using amine as starting
The block polyether class demulsifier AE8051 23g of agent, the block polyether class demulsifier BP2040 20g using alcohol as initiator, 16
Alkyl trimethyl ammonium bromide 4g, perfluorinated nonene epoxide benzene sulfonic acid sodium salt 3g, phosphoric acid 3g, methanol 5g and ethanol 42g are prepared mixed
Close alcoholic solution.
Embodiment 7
Oil-soluble composite demulsifying agent provided in this embodiment for wood tar dehydration, consisting of：Using amine as starting
Block polyether class demulsifier the AP221 20g, dodecyl benzene sulfonic acid 5g, Sodium perfluorooctanoate 5g, heavy aromatic solvent 1000# of agent
60g。
Embodiment 8
Oil-soluble composite demulsifying agent provided in this embodiment for wood tar dehydration, consisting of：Using amine as starting
The block polyether class demulsifier AE8051 17g of agent, the block polyether class demulsifier AR36 using alkyl phenolic resin as initiator
13g, isopropanol 1g, perfluorinated nonene epoxide benzene sulfonic acid sodium salt 3g, aromatic solvent 150#50g.
Embodiment 9
Composite demulsifying agent provided in this embodiment is used for the method for wood tar dehydration, its concrete operation step is as follows：
(1) wood tar raw material is taken, it is filtered, to remove solid impurity therein, then collects filtrate；
(2) composite demulsifying agent provided by the invention is added in the filtrate obtained to step (1), the addition of demulsifier is
5ppm, and be uniformly mixed at 50 DEG C；
(3) above-mentioned mixed liquor after mixing is settled, after two oil, water separation, removes water phase, that is, obtain
Dewatered wood tar.
Certainly, a kind of alternative as the present embodiment, and for different wood tar raw materials, the dosage of demulsifier
It can be adjusted with the temperature of demulsification.Also, for the higher wood tar of viscosity itself, filtering behaviour is carried out to it for convenience
Make, can be first with organic solvent, such as dimethylbenzene etc., operation of being filtered and be demulsified again after being diluted to it.
Comparative example 1
The composite demulsifying agent that this comparative example provides, consisting of：Block polyether using alkyl phenolic resin as initiator
Class demulsifier AR36 45g, perfluorinated nonene epoxide benzene sulfonic acid sodium salt 5g, aromatic solvent 150#50g。
Comparative example 2
The composite demulsifying agent that this comparative example provides, consisting of：Polyethers demulsifier DP05 25g, using alcohol as initiator
04 25g of block polyether class de-emulsifier SP, the mixture 2g of acetic acid and butanol, the mixed aqueous solution 48g of methanol and ethanol.
Comparative example 3
The composite demulsifying agent that this comparative example provides, consisting of：Block polyether class demulsifier using amine as initiator
AP221 20g, dodecyl benzene sulfonic acid 5g, Sodium perfluorooctanoate 8g, heavy aromatic solvent 1000#60g.
Comparative example 4
The composite demulsifying agent that this comparative example provides, consisting of：Block polyether class demulsifier using amine as initiator
AE8051 17g, the block polyether class demulsifier AR36 13g using alkyl phenolic resin as initiator, isopropanol 10g, perfluor nonyl
Alkenyloxy group benzene sulfonic acid sodium salt 3g, aromatic solvent 150#50g.
Comparative example 5
The Water Soluble Compound type demulsifier for being used for wood tar dehydration that this comparative example provides, consisting of：Using amine as starting
The block polyether class demulsifier AE8051 30g of agent, the block polyether class demulsifier BP2040 40g using alcohol as initiator, 16
Alkyl trimethyl ammonium bromide 4g, perfluorinated nonene epoxide benzene sulfonic acid sodium salt 3g, phosphoric acid 3g, methanol 5g and ethanol 42g are prepared mixed
Close alcoholic solution.
1 each embodiment of table and the composition of composite demulsifying agent in comparative example
Experimental example：
It is burnt that wood is carried out to the composite demulsifying agent obtained by above example 1-6 and the obtained composite demulsifying agent of comparative example
The test of oily dehydrating effect, test method are as follows：
(1) by wood tar and dimethylbenzene with volume ratio 1:1 is mixed, to be diluted to wood tar.
(2) wood tar 80ml, the distilled water 20ml after dilution are taken, above-mentioned each example demulsifier of 5ppm is injected after mixing, altogether
With adding in the tool plug graduated cylinder of 100ml, it is placed in being preheated in 80 DEG C of water bath with thermostatic control.
(3) the wood tar demulsification mixed liquor after preheating is settled.
It is another that a control group is set, demulsifier is not added, other operating procedures are identical.
Demulsification changes with time as shown in the table：
2 demulsification of table is tested
The composition of wood tar and crude oil and petroleum product differs widely, such as creosote content is higher in wood tar, including benzene
Phenol, 2- methylphenols, 4- methylphenols, 2- metoxyphenols, 3,4- xylenols, 2- ethyl -phenols etc., and in crude oil
Phenols content is relatively low.Due to wood tar complicated components, its component area with crude oil and petroleum product can not be enumerated herein
Not.The present invention is exactly the component feature for wood tar, and research and development obtain being suitable for the composite demulsifying agent of wood tar dehydration.
From experimental result as can be seen that carrying out the dehydration of wood tar using composite demulsifying agent provided by the present invention, take off
Water speed rate is considerably more rapid, and the Water Soluble Compound demulsifier that especially preferred embodiment 4-6 is provided, not only rate of water loss is obvious
Improve, dehydration quality is also more prominent.
Obviously, the above embodiments are merely examples for clarifying the description, and the restriction not to embodiment.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of change or
Change.There is no necessity and possibility to exhaust all the enbodiments.And the obvious change thus extended out or
Among changing still in protection scope of the present invention.
Claims (21)
1. a kind of composite demulsifying agent, it is characterised in that by weight, its composition includes：
20~50 parts of polyethers demulsifier, 1~5 part of auxiliary agent, 2~5 parts of fluorocarbon surfactant, 35~60 parts of solvent.
2. composite demulsifying agent according to claim 1, it is characterised in that by weight, its composition includes：Polyethers
40~50 parts of demulsifier, 2~3 parts of auxiliary agent, 3~5 parts of fluorocarbon surfactant, 40~50 parts of solvent.
3. composite demulsifying agent according to claim 1 or 2, it is characterised in that also contain in the polyethers demulsifier
One or more in anion surfactant, cationic surfactant or both sexes class surfactant.
4. according to claim 1-3 any one of them composite demulsifying agents, it is characterised in that the polyethers demulsifier includes
Block polyether using amine as initiator.
5. according to claims 1 to 3 any one of them composite demulsifying agent, it is characterised in that the polyethers demulsifier bag
Include respectively using block polyether of the amine as the block polyether of initiator and using alcohols as initiator.
6. composite demulsifying agent according to claim 5, it is characterised in that by weight, it is described respectively using amine as
The block polyether of initiator and ratio using alcohols as the block polyether of initiator are 5:4~4:5.
7. according to claims 1 to 3 any one of them composite demulsifying agent, it is characterised in that the polyethers demulsifier bag
Include respectively using block polyether of the amine as the block polyether of initiator and using alkyl phenolic resin as initiator.
8. composite demulsifying agent according to claim 7, it is characterised in that by weight, it is described respectively using amine as
The block polyether of initiator and ratio using alkyl phenolic resin as the block polyether of initiator are 5:4~4:5.
9. according to claims 1 to 3 any one of them composite demulsifying agent, it is characterised in that the polyethers demulsifier bag
Include DP classes demulsifier and the block polyether using alcohols as initiator.
10. composite demulsifying agent according to claim 9, it is characterised in that by weight, the DP classes demulsifier and
Ratio using alcohols as the block polyether of initiator is 5:4~4:5.
11. according to claim 1-10 any one of them composite demulsifying agents, it is characterised in that the auxiliary agent be solubilising,
Reagent that is scattered or adjusting one or two kinds of effects in pH value.
12. according to claim 1-11 any one of them composite demulsifying agents, it is characterised in that organic acid, inorganic acid, short branch
One or more in chain alcohol or alcohol ether.
13. composite demulsifying agent according to claim 12, it is characterised in that the organic acid is alkyl benzene sulphonate, second
One or more in acid, oxalic acid, butanedioic acid, tartaric acid, benzoic acid, caffeic acid or salicylic acid, the short-chain branch alcohol for butanol,
The mixture of isopropanol or both, the alcohol ether are isopropyl ether or ethylene glycol ethyl ether.
14. according to claim 1-13 any one of them composite demulsifying agents, it is characterised in that the fluorocarbon surfactant
For the surfactant obtained by the fluorine atom all hydrogen atom on substitution hydrocarbon chain.
15. according to claim 1-14 any one of them composite demulsifying agents, it is characterised in that the fluorocarbon surfactant
For the one or more in perfluorinated nonene base benzene sulfonic acid sodium salt, Sodium perfluorooctanoate or perfluoro-ethyl diethanol amine sodium phosphate.
16. according to claim 1-15 any one of them composite demulsifying agents, it is characterised in that the solvent is molten for oil-soluble
One or more in agent, including solvent naphtha, aromatic solvent, oil-soluble alcohol.
17. according to claim 1-16 any one of them composite demulsifying agents, it is characterised in that the solvent is water-soluble molten
One or more in agent, including water, water-soluble alcohol.
18. claim 1-17 any one of them composite demulsifying agent is used for the purposes of wood tar dehydration.
19. purposes according to claim 18, it is characterised in that the dosage of the composite demulsifying agent is 5~20ppm,
The temperature that is demulsified is 50~120 DEG C.
20. the purposes according to claim 18 or 19, it is characterised in that include the following steps：
Wood tar raw material is filtered, collects filtrate；
The filtrate is mixed with the demulsifier, obtains mixed liquor；
The mixed liquor is settled, water phase is then removed, that is, obtains dewatered wood tar.
21. according to claim 18-20 any one of them purposes, it is characterised in that before being filtered to the wood tar raw material,
First the wood tar raw material is diluted.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201810002081.7A CN108003909A (en) | 2018-01-02 | 2018-01-02 | A kind of composite demulsifying agent for wood tar dehydration |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810002081.7A CN108003909A (en) | 2018-01-02 | 2018-01-02 | A kind of composite demulsifying agent for wood tar dehydration |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112852475A (en) * | 2020-12-25 | 2021-05-28 | 天津长芦新材料研究院有限公司 | Fluorine-containing demulsifying compound and demulsifying agent for oil field |
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| CN1846830A (en) * | 2005-04-12 | 2006-10-18 | 中国科学院化学研究所 | Demulsifier |
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| CN110566816A (en) * | 2019-09-25 | 2019-12-13 | 威海翔泽新材料科技有限公司 | preparation method of tar viscosity reducer for reducing viscosity of tar |
| CN112852475A (en) * | 2020-12-25 | 2021-05-28 | 天津长芦新材料研究院有限公司 | Fluorine-containing demulsifying compound and demulsifying agent for oil field |
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Application publication date: 20180508 |