CN106336505A - Preparation method of polyether polyol - Google Patents
Preparation method of polyether polyol Download PDFInfo
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- CN106336505A CN106336505A CN201510623648.9A CN201510623648A CN106336505A CN 106336505 A CN106336505 A CN 106336505A CN 201510623648 A CN201510623648 A CN 201510623648A CN 106336505 A CN106336505 A CN 106336505A
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Abstract
The invention provides a preparation method of polyether polyol. Raw materials used in the invention comprise, by mass, 10-20 parts of mixed polyethylene glycol, 0-5 parts of glycerin, 15-40 parts of sucrose and 40-70 parts of epoxypropane. The polyether polyol is prepared through a ring opening polymerization reaction of the raw materials under the action of a catalyst, slaking and degassing. The mixed polyethylene glycol is a kettle residue in an ethylene oxide/ethylene glycol production apparatus, and is a residual raffinate obtained after extraction of ethylene glycol and diethylene glycol. The method effectively utilizes the kettle residue mixed polyethylene glycol in the ethylene oxide/ethylene glycol apparatus, saves the waste liquid treatment cost, and improves the added values of the above waste liquid. The mixed polyethylene glycol has low price, and the use amount of epoxypropane can be reduced when the polyether polyol is synthesized by adopting the mixed polyethylene glycol as an initiator, so the polyether production cost is substantially reduced, and the market competitiveness is improved.
Description
Technical field
The invention belongs to chemical field is and in particular to the preparation method of PPG.
Background technology
Mixing multiethylene-glycol is that the kettle of epoxyethane water legal production ethylene glycol technique is residual, adopts this technique domestic glycol unit more.Residual as kettle, it effective is processed and using becoming matter of utmost importance.Mixing multiethylene-glycol (i.e. multiple multicondensed ethylene glycols) is used as fuel more at present, or can respectively obtain triethylene glycol, diethylene glycol (DEG) etc. as chemical products with negative pressure simple distillation separation mixing multiethylene-glycol.Such process Land use systems Shortcomings, on the one hand do not produce higher added value, on the other hand still can produce a part of discarded object.So also will need at present preferably to mix multiethylene-glycol process Land use systems.
PPG is one of important source material of polyurethane foam.The production of existing PPG is typically based on anion catalyzed ring opening polymerization.Generally with potassium hydroxide (or NaOH), bimetallic catalyst or dimethylamine as catalyst, with the small molecule polyol such as glycerine or sucrose or other active hydrogen compoundses such as amine, hydramine as initiator, with propylene oxide (expoxy propane, abbreviation po) or propylene oxide and ethylene oxide (oxirane, abbreviation eo) mixture be monomer, carry out ring-opening polymerisation at certain temperature and pressure, obtain thick polyethers, again through the step such as neutralizing, refining, obtain polyethers finished product.The comparative maturity of existing general PPG production technology development, in recent years in order that the better quality products at good values of polyurethane material, reach the aspiration level of people, international polyurethane market increasingly trends towards exploitation and the application of the PPG to high-performance, low cost.This is accomplished by the basis of stable foam performance, the more cheap polyethers synthesizing formula of R＆D costs and technique.
In recent years, developing rapidly with polyurethane industrial, the reduction of the raising around Contents In Polyether Polyol capability and performance of domestic and international Ge great manufacturing enterprise and scientific research institution and production cost, carry out substantial amounts of research-and-development activity.Wo2007075482 reports long-chain polyether polyols.The number-average molecular weight of this long-chain polyether polyols is approximately more than 500g/mol, can be by being made with alkylene oxide to carry out alkoxylation production containing polyoxyethylated starting material in the presence of base catalyst, base catalyst has at least one and the cation containing polyoxyethylated starting material chelating.The long-chain polyether polyols of this invention can be used for providing flexible polyurethane foams and non-cellular polyurethanes.Can be used for this invention containing polyoxyethylated starting material be molecular weight be less than 500g/mol low-molecular-weight alcohol, amine, glycol, diamines, polyalcohol or the polyamines of polyether polyol initiator be can be used as by alkoxylate (with the alkylene oxide mixture of epoxy second protective embankment or the protective embankment of second containing epoxy) and prepare containing polyoxyethylated PPG.These starting materials include for example c30 single methanol, ethylene glycol, diethylene glycol (DEG), triethylene glycol, propane diols, 1, ammediol, dipropylene glycol, tripropylene glycol, neopentyl glycol, 1,4- butanediol, 1,2- butanediol, 2,3- butanediol, 1,3- butanediol, 1,6- hexylene glycol, glycerine, trimethylolpropane, trihydroxy methyl second protective embankment, pentaerythrite, D-sorbite, mannitol, hydroxymethyl glucoside, hydroxypropyl glucoside, sucrose, 1,4- cyclohexanediol, cyclohexanedimethanol, quinhydrones, resorcinol etc..
Wo2012077688 reports the manufacture method of PPG and the manufacture method of hard foamed synthetic resin.Including under conditions of no catalyst, by at least one open loop addition selected from expoxy propane and epoxy butane in the first operation of initiator, and in the presence of a catalyst at least a portion is oxirane the reaction product in the first operation for the alkylene oxide open loop addition the second operation, in the total amount of the alkylene oxide of initiator, the ratio shared by oxirane is 5%～95% for open loop addition.
Wo2012027113 reports ethylene oxide/propylene oxide PPG and the polyurethane being obtained from it.Expoxy propane and the copolymer of oxirane, its have containing 65%～90% more oxygen ethylene unit and 10%～35% oxygen propylene unit interior block, the molecular weight that this block has be 150～350.This copolymer have containing at least 95% oxygen propylene unit and 0～5% more oxygen ethylene unit outer block.The equivalent of this copolymer is 800～2000.This copolymer is useful on manufacturing the polyurethane foam with high stretching and/or tearing strength.
Cn1033522 reports a kind of synthetic method of PPG.(1) generation diethylene glycol (DEG) base glycoside is reacted with diethylene glycol (DEG) with the material with glucose ring structure, generation diethylene glycol (DEG) base glycoside PPG is polymerized under base catalyst with diethylene glycol (DEG) base glycoside and epoxides, the thick polyethers that reaction generates is neutralized reaction with nertralizer；(2) material of glucose ring structure and the weight of diethylene glycol (DEG) is than for 3: 4, and the weight of diethylene glycol (DEG) base glycoside and epoxides is than for 4: 6；(3) material of glucose ring structure and diethylene glycol (DEG) react, and range of reaction temperature is 60～200 DEG C, diethylene glycol (DEG) base glycoside and epoxide reaction, and range of reaction temperature is 80～160 DEG C.
Cn102304223 reports a kind of plant oil polyether glycol and its method of production.Including step: 15～30 parts of sucrose, 3～10 parts of diethylene glycol (DEG), 15～35 parts of soybean oil, 3～10 parts of deionized water are sequentially added in polymeric kettle by (1), it is warming up to 60～70 DEG C, stirring 0.5 hour, vacuum displacement nitrogen twice, is then evacuated to negative pressure minimum；(2) add 0.5～1.5 part of dimethylamine in polymeric kettle, stir and be warming up to 85～90 DEG C；(3) start to be passed through 10～15 parts of po, the po that second adds 30～50 parts for the first time, controlling reaction temperature is 95～105 DEG C, and < 0.3mpa, aging cooling obtains final product plant oil polyether glycol to reaction pressure.
Mixing multiethylene-glycol be oxirane glycol unit the residual product of kettle, therefore PPG is prepared by it, to not only solve the residual process problem of kettle, it is effectively utilized, more reduce the production cost of PPG, improve economic benefit.
Content of the invention
The invention provides a kind of preparation method of PPG.
Technical scheme is as follows:
A kind of preparation method of PPG, each raw material components and mass fraction are: 10～20 parts of multiethylene-glycol of mixing, 0～5 part of glycerine, 15～40 parts of sucrose, 40～70 parts of expoxy propane；Raw material, under catalyst action, by ring-opening polymerisation, cures, degassing process is obtained PPG.
Described mixing multiethylene-glycol is that the kettle of ethylene oxide/ethylene glycol process units is residual, will ethylene glycol, diethylene glycol propose after remaining raffinate, it may participate in the active principle of reaction and is mainly: ethylene glycol 0～20wt.%, diethylene glycol 0～20wt.%, triethylene glycol 10～80wt.%, tetraethylene glycol 5～40wt.%, five glycol 0～30wt.%.
Described catalyst is n, n- dimethylethanolamine, and addition is 0.2-0.8 part.
Described ring-opening polymerization temperature is 90 DEG C～130 DEG C, and pressure maintains 0.05～0.6mpa, and the ring-opening polymerization time is 3～8 hours.
Described curing temperature is 90 DEG C～130 DEG C, and pressure maintains 0.05～0.6mpa, and the curing time is 2～5 hours.
Described demonomerization temperature is 100 DEG C～130 DEG C, and vacuum is -0.1mpa, process time 2～4 hours.
Compared with prior art, advantages of the present invention is as follows:
1st, efficiently utilize the kettle raffinate mixing multiethylene-glycol of ethylene oxide/ethylene glycol plant, save the cost of liquid waste processing, improve waste liquid added value.
2nd, mixing multiethylene-glycol itself is cheap, to mix multiethylene-glycol for initiator synthesizing polyether glycol moreover it is possible to reduce the consumption of expoxy propane, greatly reduces the production cost of polyethers, improves the market competitiveness.
Specific embodiment
With reference to specific embodiment, the present invention is described in further detail.
Embodiment 1:
Multiethylene-glycol 250g, sucrose 500g, n will be mixed, n- dimethylethanolamine 5g puts in the pressure reactor of 3l stainless steel, is uniformly mixed, logical nitrogen displacement three times, is warming up to 90 DEG C, puts into po 1745g, reaction pressure is 0.2mpa, treat that po all puts in kettle, curing temperature be 90 DEG C, reaction 2 hours unchanged to pressure, then in 100 DEG C of temperature, under vacuum -0.1mpa, vacuumize removing unreacted monomer 3 hours, cooling discharge obtains inexpensive rigid-foam polyether polyol a.
Wherein: (its component is mainly 10 parts of multiethylene-glycol of mixing: ethylene glycol 20wt.%, diethylene glycol 20wt.%, triethylene glycol 20wt.%, tetraethylene glycol 30wt.%, five glycol 5wt.%), 20 parts of sucrose, 70 parts of expoxy propane, n, 0.2 part of n- dimethylethanolamine.
Embodiment 2:
Multiethylene-glycol 500g, sucrose 800g, n will be mixed, n- dimethylethanolamine 7.5g puts in the pressure reactor of 3l stainless steel, is uniformly mixed, logical nitrogen displacement three times, is warming up to 100 DEG C, puts into po 1192.5g, reaction pressure is 0.3mpa, treat that po all puts in kettle, curing temperature be 100 DEG C, reaction 3 hours unchanged to pressure, then in 110 DEG C of temperature, under vacuum -0.1mpa, vacuumize removing unreacted monomer 2 hours, cooling discharge obtains inexpensive rigid-foam polyether polyol b.
Wherein: (its component is mainly 20 parts of multiethylene-glycol of mixing: ethylene glycol 0wt.%, diethylene glycol 10wt.%, triethylene glycol 40wt.%, tetraethylene glycol 30wt.%, five glycol 10wt.%), 32 parts of sucrose, 47.7 parts of expoxy propane, n, 0.3 part of n- dimethylethanolamine.
Embodiment 3:
Multiethylene-glycol 312.5g, sucrose 675g, n will be mixed, n- dimethylethanolamine 12.5g puts in the pressure reactor of 3l stainless steel, is uniformly mixed, logical nitrogen displacement three times, is warming up to 110 DEG C, puts into po 1500g, reaction pressure is 0.1mpa, treat that po all puts in kettle, curing temperature be 110 DEG C, reaction 4 hours unchanged to pressure, then in 120 DEG C of temperature, under vacuum -0.1mpa, vacuumize removing unreacted monomer 3 hours, cooling discharge obtains inexpensive rigid-foam polyether polyol c.
Wherein: (its component is mainly 12.5 parts of multiethylene-glycol of mixing: ethylene glycol 5wt.%, diethylene glycol 10wt.%, triethylene glycol 70wt.%, tetraethylene glycol 5wt.%, five glycol 5wt.%), 27 parts of sucrose, 60 parts of expoxy propane, n, 0.5 part of n- dimethylethanolamine.
Embodiment 4:
Multiethylene-glycol 360g, sucrose 750g, n will be mixed, n- dimethylethanolamine 15g puts in the pressure reactor of 3l stainless steel, is uniformly mixed, logical nitrogen displacement three times, is warming up to 120 DEG C, puts into po 1375g, reaction pressure is 0.2mpa, treat that po all puts in kettle, curing temperature be 120 DEG C, reaction 5 hours unchanged to pressure, then in 130 DEG C of temperature, under vacuum -0.1mpa, vacuumize removing unreacted monomer 3 hours, cooling discharge obtains inexpensive rigid-foam polyether polyol d.
Wherein: 14.4 parts of multiethylene-glycol of mixing (its component is mainly: ethylene glycol 0wt.%, diethylene glycol 0wt.%, triethylene glycol 50wt.%, tetraethylene glycol 20wt.%, five glycol 20wt.%), 30 parts of sucrose, 55 parts of expoxy propane.N, n- dimethylethanolamine 0.6.
Embodiment 5:
Multiethylene-glycol 450g, sucrose 685g, n will be mixed, n- dimethylethanolamine 15g puts in the pressure reactor of 3l stainless steel, is uniformly mixed, logical nitrogen displacement three times, is warming up to 95 DEG C, puts into po1350g, reaction pressure is 0.2mpa, treat that po all puts in kettle, curing temperature be 105 DEG C, reaction 2 hours unchanged to pressure, then in 110 DEG C of temperature, under vacuum -0.1mpa, vacuumize removing unreacted monomer 3 hours, cooling discharge obtains inexpensive rigid-foam polyether polyol e.
Wherein: 18 parts of multiethylene-glycol of mixing (its component is mainly: ethylene glycol 0wt.%, diethylene glycol 5wt.%, three second two 80wt.%, tetraethylene glycol 5wt.%, five glycol 0wt.%), 27.4 parts of sucrose, 54 parts of expoxy propane, n, n- dimethylethanolamine 0.6.
Embodiment 6:
Multiethylene-glycol 300g, glycerine 25g, sucrose 1000g, n will be mixed, n- dimethylethanolamine 10g puts in the pressure reactor of 3l stainless steel, it is uniformly mixed, logical nitrogen displacement three times, it is warming up to 105 DEG C, put into po 1165g, reaction pressure is 0.4mpa, treat that po all puts in kettle, curing temperature be 100 DEG C, reaction 2 hours unchanged to pressure, then in 120 DEG C of temperature, under vacuum -0.1mpa, vacuumize removing unreacted monomer 4 hours, cooling discharge obtains inexpensive rigid-foam polyether polyol f.
Wherein: (its component is mainly 12 parts of multiethylene-glycol of mixing: ethylene glycol 0wt.%, diethylene glycol 5wt.%, three second two 35wt.%, tetraethylene glycol 40wt.%, five glycol 10wt.%), 1 part of glycerine, 40 parts of sucrose, 46.6 parts of expoxy propane, n, n- dimethylethanolamine 0.4.
Embodiment 7:
Multiethylene-glycol 425g, glycerine 50g, sucrose 375g, n will be mixed, n- dimethylethanolamine 12.5g puts in the pressure reactor of 3l stainless steel, it is uniformly mixed, logical nitrogen displacement three times, it is warming up to 115 DEG C, put into po 1637.5g, reaction pressure is 0.6mpa, treat that po all puts in kettle, curing temperature be 125 DEG C, reaction 5 hours unchanged to pressure, then in 130 DEG C of temperature, under vacuum -0.1mpa, vacuumize removing unreacted monomer 4 hours, cooling discharge obtains inexpensive rigid-foam polyether polyol g.
Wherein: (its component is mainly 17 parts of multiethylene-glycol of mixing: ethylene glycol 15wt.%, diethylene glycol 20wt.%, triethylene glycol 30wt.%, tetraethylene glycol 15wt.%, five glycol 15wt.%), 2 parts of glycerine, 15 parts of sucrose, 65.5 parts of expoxy propane, n, n- dimethylethanolamine 0.5.
Embodiment 8:
Multiethylene-glycol 280g, glycerine 75g, sucrose 565g, n will be mixed, n- dimethylethanolamine 12.5g puts in the pressure reactor of 3l stainless steel, it is uniformly mixed, logical nitrogen displacement three times, it is warming up to 110 DEG C, put into po 1567.5g, reaction pressure is 0.5mpa, treat that po all puts in kettle, curing temperature be 130 DEG C, reaction 3 hours unchanged to pressure, then in 130 DEG C of temperature, under vacuum -0.1mpa, vacuumize removing unreacted monomer 3 hours, cooling discharge obtains inexpensive rigid-foam polyether polyol h.
Wherein: (its component is mainly 11.2 parts of multiethylene-glycol of mixing: ethylene glycol 10wt.%, diethylene glycol 15wt.%, triethylene glycol 60wt.%, tetraethylene glycol 10wt.%, five glycol 0wt.%), 3 parts of glycerine, 22.6 parts of sucrose, 62.7 parts of expoxy propane, n, n- dimethylethanolamine 0.5.
Embodiment 9:
Multiethylene-glycol 325g, glycerine 100g, sucrose 425g, n will be mixed, n- dimethylethanolamine 15g puts in the pressure reactor of 3l stainless steel, it is uniformly mixed, logical nitrogen displacement three times, it is warming up to 120 DEG C, put into po 1635g, reaction pressure is 0.4mpa, treat that po all puts in kettle, curing temperature be 110 DEG C, reaction 4 hours unchanged to pressure, then in 120 DEG C of temperature, under vacuum -0.1mpa, vacuumize removing unreacted monomer 3 hours, cooling discharge obtains inexpensive rigid-foam polyether polyol i.
Wherein: (its component is mainly 13 parts of multiethylene-glycol of mixing: ethylene glycol 15wt.%, diethylene glycol 20wt.%, triethylene glycol 50wt.%, tetraethylene glycol 10wt.%, five glycol 0wt.%), 4 parts of glycerine, 17 parts of sucrose, 65.4 parts of expoxy propane, n, n- dimethylethanolamine 0.6.
Embodiment 10:
Multiethylene-glycol 432.5g, glycerine 125g, sucrose 925g, n will be mixed, n- dimethylethanolamine 17.5g puts in the pressure reactor of 3l stainless steel, it is uniformly mixed, logical nitrogen displacement three times, it is warming up to 115 DEG C, put into po 1000g, reaction pressure is 0.3mpa, treat that po all puts in kettle, curing temperature be 95 DEG C, reaction 2 hours unchanged to pressure, then in 100 DEG C of temperature, under vacuum -0.1mpa, vacuumize removing unreacted monomer 3 hours, cooling discharge obtains inexpensive rigid-foam polyether polyol j.
Wherein: (its component is mainly 17.3 parts of multiethylene-glycol of mixing: ethylene glycol 0wt.%, diethylene glycol 5wt.%, triethylene glycol 20wt.%, tetraethylene glycol 40wt.%, five glycol 30wt.%), 5 parts of glycerine, 37 parts of sucrose, 40 parts of expoxy propane, n, n- dimethylethanolamine 0.7.
Embodiment 11:
Multiethylene-glycol 432.5g, glycerine 125g, sucrose 925g, n will be mixed, n- dimethylethanolamine 17.5g puts in the pressure reactor of 3l stainless steel, it is uniformly mixed, logical nitrogen displacement three times, it is warming up to 100 DEG C, put into po 1000g, reaction pressure is 0.2mpa, treat that po all puts in kettle, curing temperature be 125 DEG C, reaction 3 hours unchanged to pressure, then in 120 DEG C of temperature, under vacuum -0.1mpa, vacuumize removing unreacted monomer 4 hours, cooling discharge obtains inexpensive rigid-foam polyether polyol k.
Wherein: (its component is mainly 19.2 parts of multiethylene-glycol of mixing: ethylene glycol 0wt.%, diethylene glycol 10wt.%, triethylene glycol 10wt.%, tetraethylene glycol 40wt.%, five glycol 30wt.%), 5 parts of glycerine, 25 parts of sucrose, 50 parts of expoxy propane, n, n- dimethylethanolamine 0.8.
The quality index of PPG a～k is listed in table 1.
Table 1 PPG analysis result
Continued 1 PPG analysis result
From table, result can be seen that, the preparation method of the PPG that this patent is proposed can synthesize qualified Contents In Polyether Polyol.
Claims (9)
1. a kind of preparation method of PPG, is characterized in that each raw material components and mass fraction are: mixing multiethylene-glycol 10～20
Part, 0～5 part of glycerine, 15～40 parts of sucrose, 40～70 parts of expoxy propane；Raw material, under catalyst action, leads to
Cross ring-opening polymerisation, curing, degassing process is obtained PPG.
2. method according to claim 1 is it is characterised in that described mixing multiethylene-glycol is ethylene oxide/ethylene glycol process units
Kettle residual, key component weight/mass percentage composition is: ethylene glycol 0～20, diethylene glycol 0～20, triethylene glycol 10～80,
Tetraethylene glycol 5～40, five glycol 0～30.
3. method according to claim 1 is it is characterised in that described catalyst is n, n- dimethylethanolamine, and addition is
0.2-0.8 part.
4. method according to claim 1 it is characterised in that described ring-opening polymerization temperature be 90 DEG C～130 DEG C, pressure
For 0.05～0.6mpa.
5. method according to claim 1 is it is characterised in that the described ring-opening polymerization time is 3～8 hours.
6. method according to claim 1 it is characterised in that described curing temperature be 90 DEG C～130 DEG C, pressure be 0.05～
0.6mpa.
7. method according to claim 1 is it is characterised in that the described curing time is 2～5 hours.
8. it is characterised in that described degassing temperature is 100 DEG C～130 DEG C, vacuum is method according to claim 1
-0.1mpa.
9. method according to claim 1 is it is characterised in that 2～4 hours described degassing process time.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107739431A (en) * | 2017-09-14 | 2018-02-27 | 江苏东邦科技有限公司 | A kind of synthesis technique of PPG as super high molecular weight resilience agent |
| CN107964074A (en) * | 2017-11-29 | 2018-04-27 | 中国石油化工股份有限公司 | A kind of preparation method of the low VOC polymer polyatomic alcohols of low cost |
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Application publication date: 20170118 |
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| RJ01 | Rejection of invention patent application after publication |