CN1023111C - Process for preparing addition products from alkyd oxides on compounds containing mobile hydrogens - Google Patents
Process for preparing addition products from alkyd oxides on compounds containing mobile hydrogens Download PDFInfo
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- CN1023111C CN1023111C CN 89106659 CN89106659A CN1023111C CN 1023111 C CN1023111 C CN 1023111C CN 89106659 CN89106659 CN 89106659 CN 89106659 A CN89106659 A CN 89106659A CN 1023111 C CN1023111 C CN 1023111C
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Abstract
Process for the preparation of an additive obtained from the condensation of an alkoxide with a compound containing mobile hydrogen, in which process the product to be condensed with the alkoxide is recycled via suitable dispersion systems of the reagent liquid in the gaseous phase of the alkoxide; the dispersion area and reaction of the liquid in the gaseous phase being separate from the collection area, preconditioning, in the said reactor, the first area above the second and suitably inclined in relation to it, as well as in relation to the ideal horizontal line.
Description
The present invention relates to a kind of promptly by making olefin oxide (the most frequently used is ethylene oxide) and compound carry out the method that condensation prepares adduct with activity or movability hydrogen with suitable catalyzer.The product that obtains therefrom has vast market, as can be used as the auxiliary in washing composition, tensio-active agent, the textile industry, poly-wet goods.
Purpose of the present invention is exactly to realize a kind of method for preparing condensation product, and the product of this method preparation is compared the quality with better character and Geng Gao with the situation that the preparation method is arranged earlier.
In fact, with compare the product that uses method of the present invention to obtain with the product of the identical ethylene oxide molecules number of having of conventional apparatus manufacturing and have much higher cloud point.
The character of this higher cloud point and improvement is relevant with narrower molecular weight distribution.
Usually compound bearing active hydrogen begins from containing in the condensation of olefin oxide, these compounds such as water, alcohol, amine, mercaptan glycerine etc.
A kind of catalyzer that is generally alkalescence of these chain material demands is as potassium hydroxide and sodium hydroxide.Sometimes can use acid catalyst, but in this case, be necessary to use special steel to build reactor.Certain recently someone has used the oxide compound or the organometallic compound of alkaline-earth metal.They are compared with traditional catalyst can obtain narrower molecular weight distribution.
The present invention does not get rid of the catalyzer of any kind, and any catalyzer all effect is fine.
Before beginning reaction, should will be present in the chaining material, in the catalyzer and catalyzer is removed with the water of chain substance reaction generation.This can reach by adopting simultaneously to vacuumize and heat at an easy rate.This mode can reduce the quantity of polyoxyethylene glycol and polypropylene glycol, and they are a kind of by products.
Reaction is carried out down and under the certain reaction pressure at 110-180 ℃ usually.The reaction pressure part is from rare gas element (being generally nitrogen), and part is from the oxide compound that reacts itself.Can adopt higher temperature for some special catalyzer.
The primitive reaction device that has agitator has a lot of shortcomings, for example, the existence of the danger of the blast that causes owing to the accumulation of unreacted dissolved oxygen thing, a large amount of polyoxyethylene glycol and the flavescence of product, speed of response is slow, and turning unit contacts with explosion gas.This device is replaced by a kind of system, and this system can make the initial substance circulation of the catalysis chain reaction that is in a liquid state, and makes the dispersion of this material in being in the gaseous oxidation thing on reactor top then.
Along with the carrying out of reaction and the increase of molecular weight, the bottom of reactor has been full of reaction product, meanwhile, reaction heat is removed by the heat exchanger in the circulation line, and ethylene oxide and/or propylene oxide directly add also evaporation herein from reactor head under control pressure become gaseous state.In order to improve the transmission of material, should increase transmission face as far as possible.
By with liquid with the form of droplet be distributed to continuous gas mutually in, can obtain very big interface, this is owing to particle much causes, reaction is just in generation at the interface.
The feature of this liquid dispersion system is: safety height when operation, and this is because the quantity of the unreacted oxide compound in liquid phase is few, and does not have rotatable parts to contact with ethylene oxide and/or propylene oxide; The speed of response height, its be agitator system 3-5 doubly; The generation of by product and color is few; And higher cloud point.
Must remember that principal reaction is to carry out on the top of reactor, herein, catalytic drop is scattered in the gas that contains oxide compound.For circulation each time, drop all has identical track and V-bar, so they have identical duration of contact, correspondingly has same rate of growth.
Therefore, in theory, in process of production, drop round-robin number of times in atmosphere surrounding is identical.Thereby compare with agitator system, can obtain the growth of quite consistent polymeric chain and narrower molecular weight distribution.
In fact, certain mixing taking place in liquid phase, makes some preferable range, closely similar with the flow reactor reactive infiltration.It is because the geometrical shape of reactor and the function of drop cause.
Purpose of the present invention is exactly that the reactor that will have vaporizer on top replaces with system of the present invention.System of the present invention has two sections, one section at the preceding paragraph down, and shape has a certain degree between them.
Therefore, new reactor is divided into two portions, and top (1) is called " liquid solid/liquid/gas reactions device "; Bottom (2) is called " retention tank ".
System representation of the present invention in the accompanying drawings, wherein 1 is " liquid solid/liquid/gas reactions device "; 2 is " retention tank "; The 3rd, recycle pump; 4,7 and 8 is heat exchangers; 5 is vacuum pump; 6 is adiabatic oil pump.
Pressure record controller and temperature recorder controller are represented by PRC and TRC respectively.
In epimere 1, reaction is always carried out under identical geometric condition from start to end, but the kinetic energy of drop is different on the valley wall of this section of reactor.
In the hypomere " retention tank " of reactor, liquid is in (liquid level increases in reaction process) under the steady state conditions, and this helps the even circulation of liquid in oxide compound atmosphere.Native system can form the more uniform circulation of reaction liquid, and has avoided the formation of advance range, and is very effective to the quality that product is provided.This can find out from the following example:
Embodiment 1
To add in the two reactor as the 2000kg nonyl phenol that contains 0.3% sodium hydroxide of catalyzer, and under recycle pump work 149 ℃ of following vacuum hydro-extractions.Then add the 4000kg ethylene oxide down and under the 5 kilograms/cm2 pressure at 180 ℃.After finishing, reaction neutralizes with the product cooling and with acetate.The OH number of the product that obtains is 85mg KOH/g, the ethylene oxide of 10 molecules that has been equivalent to condensation, and its cloud point is 68 ℃.
The cloud point of the product with identical OH number that obtains with traditional stirred reactor is 60 ℃.With having circulating evaporator, it is 64 ℃ but have only the cloud point of the product that one section reactor obtains.
Embodiment 2
To add in the two reactor as the 1800kg nonyl phenol that contains 0.34% sodium hydroxide of catalyzer, and under recycle pump work 149 ℃ of following vacuum hydro-extractions.Then add the 4320kg ethylene oxide down and under the 5 kilograms/cm2 pressure at 180 ℃.After finishing, reaction neutralizes with the product cooling and with acetate.The OH number of the product that obtains is 75mg KOH/g, the ethylene oxide of 10 molecules that has been equivalent to condensation, and its cloud point is 86 ℃.
The cloud point of the product with identical OH number that obtains with traditional stirred reactor is 78 ℃.With having circulating evaporator, it is 83 ℃ but have only the cloud point of the product that one section reactor obtains.
Embodiment 3
To add in the two reactor as the 1600kg nonyl phenol that contains 0.38% sodium hydroxide of catalyzer, and under recycle pump work 149 ℃ of following vacuum hydro-extractions.Then add the 4460kg ethylene oxide down and under the 5 kilograms/cm2 pressure at 180 ℃.After finishing, reaction neutralizes with the product cooling and with acetate.The OH number of the product that obtains is 85mgKOH/g, the ethylene oxide of 10 molecules that has been equivalent to condensation, and its cloud point is 98 ℃.
The cloud point of the product with identical OH number that obtains with traditional stirred reactor is 90 ℃.With having circulating evaporator, it is 94 ℃ but have only the cloud point of the product that one section reactor obtains.
The above embodiments and accompanying drawing all right and wrong are determinate.
Claims (4)
1, a kind of method that obtains adduct by the compound condensation that makes olefin oxide and contain the hydrogen that flows, wherein the material with the olefin oxide condensation circulates by a suitable liquid distributor, and the gas of olefin oxide mutually in reaction, the method is characterized in that before circulation and just dispersion and the reaction zone of liquid in gas phase separated with liquid collecting and storage area, and in the gas phase of reaction, do not have turning unit to contact with ethylene oxide and/or propylene oxide.
2, the method for claim 1, it is characterized in that liquid is by using one to comprise that two sections reactor reaches dispersion and the separating of reaction zone and collection and storage area in gas phase, disperse with conversion zone be positioned at store section above, so that liquid is passed through by gravity, the flowing of described liquid also have benefited from two sections each other and they and horizontal plane between a support with favored policy is arranged.
3, be used for olefin oxide and the reactor of the compound that contains the hydrogen that flows by gas liquid reaction condensation prepared adduct, described reactor comprises first case (1) of being furnished with diverting device that carries out gas liquid reaction, with second case (2) that links to each other with first case, wherein collect from the product liquid of first reaction box (1), also be furnished with circulation device described second the case, be transported in the diverting device of the 1st case (1) with the product liquid that will collect.
4, the reactor of claim 3, wherein first case (1) is positioned at second case (2) top, becomes an oblique angle with the theoretical water horizontal line, collects product liquid by gravity for two the casees.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| IT21757A/88 | 1988-08-26 | ||
| IT8821757A IT1226405B (en) | 1988-08-26 | 1988-08-26 | Process for the preparation of products with alkyd oxide additives to compounds containing mobile hydrogen |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1040784A CN1040784A (en) | 1990-03-28 |
| CN1023111C true CN1023111C (en) | 1993-12-15 |
Family
ID=11186436
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 89106659 Expired - Lifetime CN1023111C (en) | 1988-08-26 | 1989-08-26 | Process for preparing addition products from alkyd oxides on compounds containing mobile hydrogens |
Country Status (2)
| Country | Link |
|---|---|
| CN (1) | CN1023111C (en) |
| IT (1) | IT1226405B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0850954A1 (en) | 1996-12-27 | 1998-07-01 | CP TECH S.r.l. | A method for the production of polyadducts of alkylene oxides with a liquid in a gas dispersion reactor |
| HUP0001135A2 (en) * | 1997-02-25 | 2000-10-28 | Linde Ag. | A continuous process for effecting gas liquid reactions |
| CN104725169A (en) * | 2013-12-24 | 2015-06-24 | 辽宁奥克化学股份有限公司 | Method for performing alkoxylation reaction in microreactor |
| CN103739838A (en) * | 2014-01-22 | 2014-04-23 | 泰安华秦化工有限责任公司 | Method for preparing polyether polyol through external circulation spray-type reactor |
-
1988
- 1988-08-26 IT IT8821757A patent/IT1226405B/en active
-
1989
- 1989-08-26 CN CN 89106659 patent/CN1023111C/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| IT1226405B (en) | 1991-01-15 |
| CN1040784A (en) | 1990-03-28 |
| IT8821757A0 (en) | 1988-08-26 |
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Address after: Germany's Burton Patentee after: Linde AG Address before: Milan Italy Patentee before: Pressindustria S.P.A. |
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| C15 | Extension of patent right duration from 15 to 20 years for appl. with date before 31.12.1992 and still valid on 11.12.2001 (patent law change 1993) | ||
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Owner name: SD LIMITED LICENSE APPLICATION AND KG CO., LTD. Free format text: FORMER OWNER: LINDE AG. Effective date: 20050722 |
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