CN105056842B - A kind of reaction unit and its application in borate is synthesized - Google Patents
A kind of reaction unit and its application in borate is synthesized Download PDFInfo
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Abstract
A kind of reaction unit and its application in borate is synthesized, are related to reaction unit.The reaction unit is provided with preheater, reactor, products pot, condenser, byproduct tank, vacuum system：Preheater outlet connects reactor inlet by the first valve, and reactor first outlet connects products pot by the second valve, and reactor second outlet connects condenser inlet, and condensator outlet connects byproduct tank；Preheater connects vacuum system by the 3rd valve, and byproduct tank connects vacuum system by the 4th valve.Using the method for reaction unit synthesis borate：Reaction raw materials are first preheated in preheater；Raw material is delivered continuously to inside reactor in a manner of liquid pump, pressure differential or potential difference etc. in preheater, feed liquid scatter to form one layer of fluid film by reaction liquid distributor on the heating plate of inside reactor, reaction product is collected in the continuous output of reactor end outlet in products pot, accessory substance is then extracted out from reactor head, into byproduct tank.
Description
Technical field
The present invention relates to reaction unit, the application more particularly, to a kind of reaction unit and its in borate is synthesized.
Background technology
Borate type braking fluid has excellent high temperature performance, is " water non-sensitive type " brake fluid, it has also become work as previous existence
The high-performing car brake fluid that various countries of boundary competitively develop.Borate is the mostly important component of boric acid ester automobile braking fluid, it
Minor amount of water that can be in capture system is stabilized it with associated forms, so as to ensure that high-temperature behavior is unaffected.Industrial production
Borate is typically generated using boric acid and alcohol ether esterification, and acid esterification generation borate is a reversible reaction, anti-in order to promote
The positive progress answered by byproduct of reaction water, it is necessary to remove reaction system in time.
The esterification that patent CN101735254B is catalyzed inorganic boric acid and alcohol using acid chaotropic body as catalysts and solvents is anti-
Should, obtain borate.For patent CN102796600A using high polyalcohol ether, boric acid, propane diols as raw material, two sections of esterification process have synthesized one
The hexatomic ring borate of kind low-viscosity, improve the dry equilibrium boiling point and hydrolytic stability of brake fluid.Need nitrogen protection, toluene
Band water, esterification time 2-4h.These methods use solvent, the problems such as cost height, later separation step complexity, industry be present
It is more difficult to change application.
Patent CN102031179B proposes a kind of method for preparing borate in non-isothermal transformation dynamic response technique, should
Method using non-isothermal transformation dynamic response condition make more glycol ethers of three boron oxygen keys in boric acid and different molecular weight by
Step combines, and synthesizes the borate with three different ester groups.What patent CN103333188A was passed through by boric acid and continuously
Alcohol ether carries out esterification, vacuumizes, the distillate and borate separated.Distillate is divided water and alcohol ether by distillation
From.Patent CN102618354B is by ethylene glycol mono-ether, ethylene glycol or polyethylene glycol, boric acid, diluent, pH adjusting agent and corrosion inhibiter
Put into proportion in reactor, open vavuum pump and heater, 1h is respectively incubated in 60-100 DEG C and 140-160 DEG C of temperature section,
Pump reaction of moisture to terminate, obtain faint yellow borate.These patents are first to be carried out at a lower temperature in batch still
The reaction of a period of time, then extract water byproduct out from reaction system under high temperature high vacuum condition.This method is in high temperature Gao Zhen
Some lower boiling alcohol ethers materials can be caused to be extracted reaction system together during pumping water byproduct under empty condition, sternly
The yield of reaction is reduced again, and the borate product higher to obtain dry and wet boiling point, product also need to carry by rectifying column
It is pure, the shortcomings of high energy consumption, reaction time is long, product turns to be yellow be present, seriously constrain borate-type basal liquid and high-performance braking
The development of liquid.
The content of the invention
It is an object of the invention to provide achievable rapidly, continuously esterification, and obtain stable prod, increase reaction and
Area is dehydrated, realizes reaction and a kind of reaction unit for dividing water while carrying out.
Another object of the present invention is to provide application of the reaction unit in borate is synthesized.
The reaction unit is provided with preheater, reactor, products pot, condenser, byproduct tank, vacuum system：Preheater
Outlet connects reactor inlet by the first valve, and reactor first outlet connects products pot by the second valve, and reactor second goes out
Mouth connects condenser inlet, and condensator outlet connects byproduct tank；Preheater connects vacuum system by the 3rd valve, and byproduct tank passes through
4th valve connects vacuum system.
The preheater can use still preheater.
In the reactor be provided with can temperature control heating plate, heating plate connection vacuum system, formed vacuum.And heating plate
Inclination angle can be varied as desired in, so as to change the flowing of reaction liquid material above heating plate (including such as the residence time, reaction solution
Film thickness).
Fin, groove etc. can be provided with the heating plate, is uniformly distributed on hot plate for reaction solution；The heating plate
Electric boiling plate or reaction bed can be used, tile solid catalyst on the reaction bed.
Method using reaction unit synthesis borate comprises the following steps：
1) reaction raw materials are first preheated in preheater；
2) raw material is delivered continuously to inside reactor, feed liquid in a manner of liquid pump, pressure differential or potential difference etc. in preheater
It scatter to form one layer of fluid film on the heating plate of inside reactor by reaction liquid distributor, reaction product is anti-
The continuous output of device end outlet is answered to be collected in products pot, accessory substance is then extracted out from reactor head, into byproduct tank.
In step 1), the reaction raw materials are boric acid and all kinds of alcohol ethers or alcohol-ether mixture, and wherein alcohol ether may be selected from
More gylcol ether or polyalcohols ethers etc., more gylcol ethers may be selected from triethylene glycol methyl ether, triethylene glycol butyl ether etc.
One kind, the polyalcohols ethers may be selected from one kind in polyethylene glycol, methoxypolyethylene glycol etc.；The mol ratio of alcohol ether and boric acid can
For (2~5): 1；The preheater can be normal pressure or vacuum state, and the temperature of the preheating can be 50~150 DEG C.
In step 2), fin, groove etc. can be provided with the heating plate, heating plate is evenly distributed on for reaction solution
On；The heating plate can use electric boiling plate or reaction bed, and tile solid catalyst on the reaction bed；The temperature of heating plate can
For 140~250 DEG C；The vacuum of the reactor can be 0.08~0.1MPa.
In order to realize rapidly, continuously esterification, and obtain stable prod.The present invention proposes a kind of continuous reaction device
The method for synthesizing borate：Liquid reactions material is entered in tubular reactor after preheating, forms one layer in the reactor
Fluid film, reaction and dehydration area are increased, realizes reaction and the continuous esterification for dividing water while carrying out.
Using the reaction unit, serialization is quickly esterified and divides the new technique for synthesizing of water.That is, raw material is allowed to first pass through
Preheating, then by the high-temperature heating plate in reactor, raw material disperses and forms one layer of reaction liquid film on hot plate, so as to improve
Reaction solution degree of being heated evenly simultaneously increases reaction solution disengagement area so that water byproduct caused by esterification can be easier from anti-
Answer in system and separate, and then realize quick esterification and continuous production.
The method that the present invention is esterified using reaction unit, is dehydrated.The reaction unit is furnished with controllable temperature heating plate, adds
Hot plate is provided with the reaction liquid distributors such as fin, groove and can have catalyst, so that reaction solution thermally equivalent reacts, and
Substantially increase response area.The cavity of certain space size above reaction liquid level can vacuumize so that be evaporated in reaction solution
Moisture content out etc. realizes quick removal because disengagement area is big.Design ensure that the quick progress of esterification above, and can
Realize from the continuous production for being fed to discharging.The present invention solves the lactate synthesis process of batch reactor used by tradition
Caused by course of reaction relies on strong stirring, high energy consumption, length reaction time, uneven heating the shortcomings of poor product quality, closed in ester
There is significant advantage and application prospect on into technique.
The maximum feature of the present invention is to make reaction mass form one layer of liquid film in the reactor to be reacted, and increases reaction
Area, make accessory substance be more easy to separate from reaction system, improve reaction conversion ratio, improve reaction efficiency, reduce
Product time of contact at high temperature, there is provided product quality, and the serialization of process, scale can be realized.
Brief description of the drawings
Fig. 1 is the structure composition schematic diagram of reaction unit of the present invention.
In Fig. 1, each mark for：E-1 reactors (dash area is heating plate)；E-2 still preheaters；E-3 products pots；E-4
Byproduct tank；E-5 condensers；P1 pressure display tables；The temperature controls of T1 first and display table, T2 second temperatures control and display
Table；The valves of V-1 first, the valves of V-2 second, the valves of V-3 the 3rd, the valves of V-4 the 4th, A vacuum systems.
Embodiment
With reference to embodiment, the invention will be further described, but present invention protection content is not limited only to this.
Referring to Fig. 1, the reaction unit embodiment is provided with still preheater E-2, reactor E-1, products pot E-3, condenser E-
5th, byproduct tank E-4, vacuum system A：Still preheater E-2 outlets meet reactor E-1 entrances, reactor E-1 by the first valve V-1
First outlet meets products pot E-3 by the second valve V-2, and reactor E-1 second outlets meet condenser E-5 entrances, condenser E-5
Outlet meets byproduct tank E-4；Still preheater E-2 meets vacuum system A by the 3rd valve V-3, and byproduct tank E-4 passes through the 4th valve
V-4 meets vacuum system A.
In the reactor be provided with can temperature control heating plate, heating plate connection vacuum system, formed vacuum.And heating plate
Inclination angle can be varied as desired in, so as to change the flowing of reaction liquid material above heating plate (including such as the residence time, reaction solution
Film thickness).
Fin, groove etc. can be provided with the heating plate, is uniformly distributed on hot plate for reaction solution；The heating plate
Electric boiling plate or reaction bed can be used, tile solid catalyst on the reaction bed.
The embodiment of the method given below that borate is synthesized using the reaction unit：
Embodiment 1
Medicine：Triethylene glycol methyl ether (Jiangsu Tianyin chemical Co., Ltd, technical grade), (fringe glad chemical industry in Guangzhou is limited for boric acid
Company, purity >=99.0%).
Preparation work：9.7g boric acid and 90.3g triethylene glycol methyl ethers are mixed, 80 DEG C of constant temperature stirrings in still preheater
30min。
It is 0.098MPa that the first step, which keeps tubular reaction vessel vacuum, and temperature of heating plate is 160 DEG C in tubular reaction vessel, logical
Liquid pump is crossed to get to reaction mass in reactor from still preheater (feed rate about 10mL/min).
Second step carries out continuous blowing by observing liquid film state in tubular reaction vessel.
The index of reacted product detection is as follows：Dry boiling point：283 DEG C, wet boiling point：205 DEG C, -40 DEG C of kinematic viscosity：
1249mm2/s。
Embodiment 2
Medicine：Triethylene glycol methyl ether (Jiangsu Tianyin chemical Co., Ltd, technical grade), (fringe glad chemical industry in Guangzhou is limited for boric acid
Company, purity >=99.0%).
The present embodiment uses the step as embodiment 1, unlike:Heating plate temperature in tubular reaction vessel in the first step
Spend for 180 DEG C.
The index of reacted product detection is as follows：Dry boiling point：289 DEG C, wet boiling point：208 DEG C, -40 DEG C of kinematic viscosity：
1257mm2/s。
Embodiment 3
Medicine：Triethylene glycol methyl ether (Jiangsu Tianyin chemical Co., Ltd, technical grade), (fringe glad chemical industry in Guangzhou is limited for boric acid
Company, purity >=99.0%).
The present embodiment uses the step as embodiment 1, unlike:Preparation work still preheater for 60 DEG C.
The index of reacted product detection is as follows：Dry boiling point：271 DEG C, wet boiling point：199 DEG C, -40 DEG C of kinematic viscosity：
1196mm2/s。
Embodiment 4
Medicine：Triethylene glycol methyl ether (Jiangsu Tianyin chemical Co., Ltd, technical grade), (fringe glad chemical industry in Guangzhou is limited for boric acid
Company, purity >=99.0%).
The present embodiment uses the step as embodiment 1, unlike:Feed rate in the first step is 18mL/
Min, temperature of heating plate are 200 DEG C.
The index of reacted product detection is as follows：Dry boiling point：279 DEG C, wet boiling point：203 DEG C, -40 DEG C of kinematic viscosity：
1233mm2/s。
Embodiment 5
Medicine：Triethylene glycol methyl ether (Jiangsu Tianyin chemical Co., Ltd, technical grade), (fringe glad chemical industry in Guangzhou is limited for boric acid
Company, purity >=99.0%).
The present embodiment uses the step as embodiment 1, unlike:The vacuum of tubular reaction vessel is in the first step
0.096MPa。
The index of reacted product detection is as follows：Dry boiling point：280 DEG C, wet boiling point：203 DEG C, -40 DEG C of kinematic viscosity：
1235mm2/s。
Embodiment 6
Medicine：Triethylene glycol butyl ether (Jiangsu Tianyin chemical Co., Ltd, technical grade), (fringe glad chemical industry in Guangzhou is limited for boric acid
Company, purity >=99.0%).
The present embodiment uses the step as embodiment 1, unlike:The raw material reacted in preparation work is three second two
Alcohol butyl ether, and addition is 113g.
The index of reacted product detection is as follows：Dry boiling point：290 DEG C, wet boiling point：201 DEG C, -40 DEG C of kinematic viscosity：
1280mm2/s。
Embodiment 7
Medicine：Polyethylene glycol (Jiangsu Tianyin chemical Co., Ltd, technical grade), boric acid (Guangzhou Sui Xin Chemical Co., Ltd.s,
Purity >=99.0%).
The present embodiment uses the step as embodiment 1, unlike:The raw material reacted in preparation work is poly- second two
Alcohol, and addition is 120g.
The index of reacted product detection is as follows：Dry boiling point：310 DEG C, wet boiling point：209 DEG C, -40 DEG C of kinematic viscosity：
1410mm2/s。
Claims (7)
1. a kind of reaction unit, it is characterised in that provided with preheater, reactor, products pot, condenser, byproduct tank, vacuum system
System：Preheater outlet connects reactor inlet by the first valve, and reactor first outlet connects products pot by the second valve, reaction
Device second outlet connects condenser inlet, and condensator outlet connects byproduct tank；Preheater connects vacuum system by the 3rd valve, by-product
Product tank connects vacuum system by the 4th valve；
In the reactor be provided with can temperature control heating plate, heating plate connection vacuum system, formed vacuum.
2. a kind of reaction unit as claimed in claim 1, it is characterised in that the preheater uses still preheater.
3. a kind of reaction unit as claimed in claim 2, it is characterised in that the heating plate is provided with fin, groove.
4. a kind of reaction unit as described in claim 1 or 3, it is characterised in that the heating plate uses electric boiling plate or reaction
Bed, tile solid catalyst on the reaction bed.
5. the method for application reaction unit synthesis borate as described in any in Claims 1 to 4, it is characterised in that including following
Step：
1) reaction raw materials are first preheated in preheater；
The reaction raw materials are boric acid and all kinds of alcohol ethers or alcohol-ether mixture, and wherein alcohol ether is selected from more gylcol ethers or polyalcohols
Ethers, the one kind of more gylcol ethers in triethylene glycol methyl ether, triethylene glycol butyl ether, the polyalcohols ethers are selected from poly-
One kind in ethylene glycol, methoxypolyethylene glycol；The mol ratio of alcohol ether and boric acid is (2~5): 1；
2) raw material is delivered continuously to inside reactor in a manner of liquid pump, pressure differential or potential difference etc. in preheater, and feed liquid passes through
Reaction liquid distributor scatter to form one layer of fluid film on the heating plate of inside reactor, and reaction product is in reactor
The continuous output of end outlet is collected in products pot, and accessory substance is then extracted out from reactor head, into byproduct tank.
6. method as claimed in claim 5, it is characterised in that the preheater is normal pressure or vacuum state, the temperature of the preheating
Spend for 50~150 DEG C.
7. method as claimed in claim 5, it is characterised in that in step 2), the temperature of the heating plate is 140~250 DEG C；
The vacuum of the reactor is 0.08~0.1MPa.
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| CN1048542A (en) * | 1989-07-03 | 1991-01-16 | 天津石油化工公司化工厂 | A kind of production method of dimethyl terephthalate (DMT) |
| US20060173157A1 (en) * | 2003-03-31 | 2006-08-03 | Toshio Endo | Lactone polyester polyols and process for production thereof |
| CN101265184B (en) * | 2007-03-12 | 2010-09-01 | 中国石油天然气股份有限公司 | Method for preparing dibasic acid ester |
| CN101318969A (en) * | 2007-06-07 | 2008-12-10 | 南通鸿志化工有限公司 | Distillation method for preparing high-purity trimethyl borate |
| CN101575347B (en) * | 2009-06-16 | 2011-06-01 | 江苏龙蟠石化有限公司 | Method for preparing bridge borate lubricating agent |
| CN103827124B (en) * | 2011-09-14 | 2017-06-06 | 陶氏益农公司 | Method and system for forming boric acid class and its intermediate |
| CN102618354B (en) * | 2012-03-08 | 2013-06-26 | 中国船舶重工集团公司第七一八研究所 | Method for preparing borate synthetic brake fluid |
| CN103073728A (en) * | 2012-04-01 | 2013-05-01 | 张曦 | Boron-containing polyester, and synthesizing method and applications thereof |
| CN103333188B (en) * | 2013-07-25 | 2016-06-08 | 中国石油化工股份有限公司 | A kind of production method of borate |
| CN203768336U (en) * | 2014-04-09 | 2014-08-13 | 南京华阜尚研能源科技有限公司 | Efficient esterification and interesterification reaction device |
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Effective date of registration: 20190613 Address after: 361000 Mao Xue Guangshe 398, Yongyao Village, Haicang District, Xiamen City, Fujian Province Patentee after: XIAMEN WONRKA LUBRICANT CO., LTD. Address before: Xiamen City, Fujian Province, 361005 South Siming Road No. 422 Co-patentee before: XIAMEN WONRKA LUBRICANT CO., LTD. Patentee before: Xiamen University |