CN109183089A - A kind of one one step preparation method of propine alcohol ethoxylates and its application - Google Patents

A kind of one one step preparation method of propine alcohol ethoxylates and its application Download PDF

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Publication number
CN109183089A
CN109183089A CN201810961349.XA CN201810961349A CN109183089A CN 109183089 A CN109183089 A CN 109183089A CN 201810961349 A CN201810961349 A CN 201810961349A CN 109183089 A CN109183089 A CN 109183089A
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alcohol ethoxylates
propine
step preparation
reaction
propine alcohol
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Inventor
任凡
王亮
王杰
张静
刘治田
张旗
耿聪
付远波
程宝
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Wuhan Oxiran Specialty Chemicals Co
Wuhan Institute of Technology
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Wuhan Oxiran Specialty Chemicals Co
Wuhan Institute of Technology
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00Electroplating: Baths therefor
    • C25D3/02Electroplating: Baths therefor from solutions
    • C25D3/12Electroplating: Baths therefor from solutions of nickel or cobalt
    • C25D3/14Electroplating: Baths therefor from solutions of nickel or cobalt from baths containing acetylenic or heterocyclic compounds
    • C25D3/16Acetylenic compounds

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Catalysts (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Electroplating And Plating Baths Therefor (AREA)

Abstract

The invention discloses an a kind of one step preparation method of propine alcohol ethoxylates and its application, the propine alcohol ethoxylates are obtained by propilolic alcohol and ethylene oxide synthesis.Specifically: propilolic alcohol and quaternary ammonium alkali catalyst are added in reaction kettle, it carries out multiple nitrogen displacement and vacuumizes, then pass to ethylene oxide, controlling reaction temperature is 82~88 DEG C, reaction pressure is 0.3MPa~0.5MPa, finally carries out post-processing aging to product, maintains aforesaid reaction vessel temperature, until reactor pressure no longer declines, it is down to and is neutralized after 60 DEG C with glacial acetic acid and take off low boiling.The propine alcohol ethoxylates of one-step method preparation have many advantages, such as high conversion rate, acetylene bond retention rate are high, of light color, can substitute original mode for needing distilation, substantially reduce the amount of waste, more environmentally protective compared to preparation method before.The propine alcohol ethoxylates are applied in electro-nickel process, obtained coating is full, substantially without plating leakage.

Description

A kind of one one step preparation method of propine alcohol ethoxylates and its application
Technical field
The present invention relates to a kind of preparations of a step of nickel plating brightener technical field more particularly to propine alcohol ethoxylates Method and its application.
Background technique
Brightener is developed so far the history of existing decades, is as one of chemical plating, the adding ingredient of plating.It can make Coating is uniform, and it is decorative to improve plating piece.In terms of protective value, it can improve the corrosion resistance of product, and improve service life. In terms of functionality, the specific functions such as wearability, the greasy property of workpieces processing can be improved.
Brightener is divided into macroscopical dispersibility improver i.e. smooth agent according to the difference of effect, and microcosmic dispersibility changes Kind agent (leveling agent), wetting agent, modifying agent (functional additive), screening agent, adjuvant.The effect difference of each additive is as follows It is described.
1. brightener is the additive for the purpose of obtaining bright property coating.2. smooth agent is to improve coating dispersion energy Power, to make coating crystallize careful additive.3. leveling agent is the additive for the purpose of obtaining smooth coating.4. wetting agent It is to make hydrogen be easy to overflow and reduce the additive of pin hole to reduce electrolyte surface tension.5. being answered to improve in coating The additive of power, hardness, toughness or other function.6. this in order to exclude the influence of micro reluctant impurity addition masking The additive of impurity.7. adjuvant is used together to increase the effect of other Additives or add with other with other additives Agent is added to be used together the additive that could play effect.
Nickel plating brightener is developed so far, and experienced four-stage: the first stage is to use inorganic brightener, such as cadmium salt; Second stage is alkynol and saccharin;Phase III is the condensation product and saccharin of alkynol and epoxide;Fourth stage is centre The second-class brightener of body compounding and the softening agent as primary brightener, i.e., so-called forth generation nickel plating brightener.
Wherein propine alcohol ethoxylates are as common electronickelling brightener, and quickly to go out light, decomposition product is few, use The advantages that amount is few largely uses.
Chinese invention patent (application number: 200810029477.7 applyings date: 2008-07-15) discloses 4- hydroxyl -2- fourth The preparation method of alkynyl -2- hydroxyalkyl ether nickel plating intermediate, the preparation method announced is only applicable to small trial production, not to distillation Purifying technique is described, and uses traditional sodium hydroxide that cannot reach the operation for removing distillation from.
Chinese invention patent (application number: 201510738184.6 applyings date: 2015-11-03) discloses a kind of 1- propine The synthetic method of base glycerol ether, and clearly propose to need to depressurize to steam to solution temperature in the patent to rise recycling propilolic alcohol, it obtains First step intermediate, while needing to be concentrated under reduced pressure into most of water and steaming.There are biggish safety winds for propilolic alcohol for this Danger.
Hunan University Zhang Yue has carried out in detail propilolic alcohol and Isosorbide-5-Nitrae-butynediols synthesising process research in its Master's thesis Thin general introduction also illustrates that acetylenic substance is unstable, be easy to appear explosion etc. danger, so remove from distillation not only can environmental protection simultaneously Security risk can be greatly reduced.
It, all can not the safety of physical presence or green one in very good solution production process compared to patent mentioned above The problem of step synthesis, many limitations are faced with using traditional handicraft.
Summary of the invention
Based on the above the deficiencies in the prior art, technical problem solved by the invention is to provide a kind of propine alcohol ethoxy The propine alcohol ethoxylates of one one step preparation method of compound and its application, one-step method preparation have high conversion rate, alkynes Many advantages, such as key retention rate is high, of light color, can substitute original mode for needing distilation, substantially reduce waste Amount, it is more environmentally protective compared to preparation method before.
In order to solve the above technical problem, the present invention provides an a kind of one step preparation method of propine alcohol ethoxylates, Specifically: propilolic alcohol and quaternary ammonium alkali catalyst is added in the autoclave with stirring of 1L, air-tightness inspection is carried out to reaction kettle It looks into, nitrogen displacement and vacuum pumping is carried out to it under the conditions of 50 DEG C after there is not pressure phenomenon in reaction kettle 1h, really The pumpdown time is protected greater than 30min, high pure nitrogen is replaced 5 times, then row pressure to 0~30KPa is passed through epoxy second into reaction kettle Alkane, control reaction temperature is 85 DEG C ± 3 DEG C and reaction pressure is 0.3MPa~0.5MPa, until the total amount for being passed through ethylene oxide is Stop being passed through ethylene oxide when 10mol, product is carried out post-processing aging to maintain temperature of reaction kettle being 85 DEG C ± 3 DEG C, until anti- It answers kettle pressure no longer to decline, shows to complete slaking reaction.60 DEG C are down to, is neutralized with glacial acetic acid.
As a preferred embodiment of the above technical solution, an one step preparation method of propine alcohol ethoxylates provided by the invention into One step includes some or all of following technical characteristic:
As an improvement of the above technical solution, the quaternary ammonium alkali catalyst includes tetramethylammonium hydroxide, tetraethyl hydrogen One or more of amine-oxides, tetrapropylammonium hydroxide, tetrabutylammonium hydroxide.
As an improvement of the above technical solution, the additive amount of the quaternary ammonium alkali catalyst is the 0.05~2% of gross mass.
The ethoxymer distribution, the i.e. degree of polymerization are 0.5~6mol.
The above problem can also be achieved through the following technical solutions: a kind of application of propine alcohol ethoxylates, described Propine alcohol ethoxylates are used as nickel plating brightener, specifically used method are as follows: in 250~300g/L of nickel sulfate, nickel chloride 50 ~60g/L, 40~50g/L of boric acid basal liquid in, be added 1~2g/L of saccharin sodium, add propine alcohol ethoxylate 0.01 ~0.03g/L, at 50~60 DEG C, 3~5A/dm of cathode-current density2Under be electroplated.
Compared with prior art, technical solution of the present invention, which has the following beneficial effects:, solves following technical problem:
First technical problem is that preparation method of the present invention not only overcomes traditional inorganic base catalyst color Problem deep, alkynyl retention rate is low, and it is more environmentally protective.
Such as due to traditional inorganic base catalyst: potassium hydroxide and sodium hydroxide are easy to cause alkynol substance to decompose reduction alkynes Base retention rate, decomposition while, will lead to color burn, while propilolic alcohol is easy to oxidize under basic conditions that catalyst is made to lose work Property, cause synthesis to occur dangerous, and the relatively low hot conditions for generally requiring 100 DEG C or more of catalytic activity could be catalyzed well Synthesis, is unfavorable for the narrow ditribution of ethylene oxide under these conditions.It needs to use distillation decoloration since color is too deep, and distills de- Color will bring various three wastes problems, more environmentally protective compared to this technique of traditional handicraft.
Second technical problem is to provide one kind in lower temperature range, by the nitrogenous class catalyst of high activity come The method for realizing narrow ditribution effect.
Organic alkali quaternary ammonium alkali catalyst with steric hindrance has many excellent characteristics, relative to organic fatty Amine its do not allow it is oxidizable, while alkalinity compared with by force ethoxylation synthesis in catalytic effect it is particularly evident, just because of this characteristic So that organic alkali quaternary ammonium alkali catalyst can carry out ethoxylation synthetic reaction under lower temperature conditions, it is also narrow Distribution is laid a good foundation.
Third technical problem, being that the sample that conventional catalyst synthesis is solved by narrow ditribution needs to distill can be only achieved The problem of purity requirement.Realize one-step synthesis, three-waste free discharge.Traditional handicraft distills bring security risk and waste water, gives up Slag etc. is difficult to handle, and preparation method of the invention can substitute original mode for needing distilation, substantially reduces waste Amount.
Traditional catalyst inorganic base and fatty amine catalysate contain a large amount of unreacted third since molecular weight distribution is wider Alkynol and other by-products, this kind of by-product is unfavorable to nickel plating, while the purity reduction of product will make product without competing Striving power can not be with same kind of products at abroad to matching in excellence or beauty, and the present invention uses the nitrogenous class catalyst of large space steric hindrance can be with single sintering just It can achieve with same kind of products at abroad to matching in excellence or beauty, remove distillation technique from, shorten process flow, reduction while having saved energy consumption Real greenization production has been accomplished in the discharge of waste water and dregs.
4th technical problem is the distribution character of improvement product, improves the narrow ditribution characteristic of product.Improve product Application effect.
Using the organic alkali quaternary ammonium salt catalyst with steric hindrance due to its space steric effect, can influence to produce The distribution of epoxy adduct number in product, and then enhance product performance.The alkane with narrow ditribution characteristic supports based compound tool in general There is more excellent performance, this product is also related with molecular weight distribution width, and relatively narrow properties of product are more excellent.
The above description is only an overview of the technical scheme of the present invention, in order to better understand the technical means of the present invention, And it can be implemented in accordance with the contents of the specification, and in order to allow above and other objects, features and advantages of the invention can It is clearer and more comprehensible, below in conjunction with preferred embodiment, detailed description are as follows.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, the attached drawing to embodiment is simply situated between below It continues.
The schematic diagram of the plating piece of nickel coating prepared by Fig. 1 embodiment of the present invention 6 and embodiment 10;
Fig. 2 is the schematic diagram of the plating piece of nickel coating prepared by inventive embodiments 6 and embodiment 9;
Fig. 3 is to have used the embodiment of the present invention 6 (the optimal synthetic schemes filtered out) and 10 phase knot of embodiment from top to bottom The plating piece knot that plating piece result, the old technique that plating piece result, the old technique of conjunction are combined with embodiment 9 are combined with embodiment 10 The signal of propine alcohol ethoxylates plating piece prepared by the plating piece result that fruit, product on the market are combined with embodiment 10 Figure.
Specific embodiment
The following detailed description of a specific embodiment of the invention, as part of this specification, by embodiment come Illustrate that the principle of the present invention, other aspects of the present invention, feature and its advantage will become apparent by the detailed description.
Embodiment 1
The propilolic alcohol and 5g tetramethylammonium hydroxide of 5mol are added in the autoclave with stirring of 1L, reaction kettle is carried out Airtight test carries out nitrogen displacement to it under the conditions of 50 DEG C after there is not pressure phenomenon in reaction kettle 1h and vacuumizes Operation, it is ensured that the pumpdown time is greater than 30min, high pure nitrogen displacement number of operations 5 times, row pressure to 0~30KPa, then to anti- It answers and is passed through ethylene oxide in kettle, control reaction temperature is 85 DEG C ± 3 DEG C and reaction pressure is 0.3MPa~0.5MPa, until being passed through Stop being passed through ethylene oxide when the total amount of ethylene oxide is 10mol, carrying out post-processing aging maintenance temperature of reaction kettle to product is 85 DEG C ± 3 DEG C, until reactor pressure no longer declines, show to complete slaking reaction.60 DEG C are down to, is neutralized with glacial acetic acid.
Prepared propine alcohol ethoxylates are used as nickel plating brightener, then measure the plating piece performance of product and right Than selecting optimal case.
Embodiment 2
The propilolic alcohol of addition 5mol and 5g tetramethylammonium hydroxide and tetraethyl hydrogen-oxygen in the autoclave with stirring of 1L Change ammonium mixture (mixture quality ratio is 1:3), airtight test is carried out to reaction kettle, to not occur pressure in reaction kettle 1h Nitrogen displacement and vacuum pumping are carried out to it under the conditions of 50 DEG C after phenomenon, it is ensured that the pumpdown time is greater than 30min, High Purity Nitrogen Then gas displacement number of operations 5 times, row pressure to 0~30KPa are passed through ethylene oxide into reaction kettle, control reaction temperature is 85 DEG C ± 3 DEG C and reaction pressure are 0.3MPa~0.5MPa, until the total amount for being passed through ethylene oxide stops being passed through epoxy when being 10mol Ethane carries out post-processing aging to maintain temperature of reaction kettle being 85 DEG C ± 3 DEG C to product, until reactor pressure no longer declines, table Bright completion slaking reaction.60 DEG C are down to, is neutralized with glacial acetic acid and takes off low boiling.
Prepared propine alcohol ethoxylates are used as nickel plating brightener, then measure the plating piece performance of product and right Than selecting optimal case.
Embodiment 3
The propilolic alcohol and 5g tetraethyl ammonium hydroxide of 5mol are added in the autoclave with stirring of 1L, reaction kettle is carried out Airtight test carries out nitrogen displacement to it under the conditions of 50 DEG C after there is not pressure phenomenon in reaction kettle 1h and vacuumizes Operation, it is ensured that the pumpdown time is greater than 30min, high pure nitrogen displacement number of operations 5 times, row pressure to 0~30KPa, then to anti- It answers and is passed through ethylene oxide in kettle, control reaction temperature is 85 DEG C ± 3 DEG C and reaction pressure is 0.3MPa~0.5MPa, until being passed through Stop being passed through ethylene oxide when the total amount of ethylene oxide is 10mol, carrying out post-processing aging maintenance temperature of reaction kettle to product is 85 DEG C ± 3 DEG C, until reactor pressure no longer declines, show to complete slaking reaction.60 DEG C are down to, neutralized with glacial acetic acid and is taken off are low Boiling.
Prepared propine alcohol ethoxylates are used as nickel plating brightener, then measure the plating piece performance of product and right Than selecting optimal case.
Embodiment 4
The propilolic alcohol and 5g tetrapropylammonium hydroxide of 5mol are added in the autoclave with stirring of 1L, reaction kettle is carried out Airtight test carries out nitrogen displacement to it under the conditions of 50 DEG C after there is not pressure phenomenon in reaction kettle 1h and vacuumizes Operation, it is ensured that the pumpdown time is greater than 30min, high pure nitrogen displacement number of operations 5 times, row pressure to 0~30KPa, then to anti- It answers and is passed through ethylene oxide in kettle, control reaction temperature is 85 DEG C ± 3 DEG C and reaction pressure is 0.3MPa~0.5MPa, until being passed through Stop being passed through ethylene oxide when the total amount of ethylene oxide is 10mol, carrying out post-processing aging maintenance temperature of reaction kettle to product is 85 DEG C ± 3 DEG C, until reactor pressure no longer declines, show to complete slaking reaction.60 DEG C are down to, neutralized with glacial acetic acid and is taken off are low Boiling.
Prepared propine alcohol ethoxylates are used as nickel plating brightener, then measure the plating piece performance of product and right Than selecting optimal case.
Embodiment 5
The propilolic alcohol of addition 5mol and 5g tetramethylammonium hydroxide and tetraethyl hydrogen-oxygen in the autoclave with stirring of 1L Change ammonium mixture (mixture quality ratio is 1:3), airtight test is carried out to reaction kettle, to not occur pressure in reaction kettle 1h Nitrogen displacement and vacuum pumping are carried out to it under the conditions of 50 DEG C after phenomenon, it is ensured that the pumpdown time is greater than 30min, High Purity Nitrogen Then gas displacement number of operations 5 times, row pressure to 0~30KPa are passed through ethylene oxide into reaction kettle, control reaction temperature is 85 DEG C ± 3 DEG C and reaction pressure are 0.3MPa~0.5MPa, until the total amount for being passed through ethylene oxide stops being passed through epoxy when being 10mol Ethane carries out post-processing aging to maintain temperature of reaction kettle being 85 DEG C ± 3 DEG C to product, until reactor pressure no longer declines, table Bright completion slaking reaction.60 DEG C are down to, is neutralized with glacial acetic acid and takes off low boiling.
Prepared propine alcohol ethoxylates are used as nickel plating brightener, then measure the plating piece performance of product and right Than selecting optimal case.
Embodiment 6
The propilolic alcohol of addition 5mol and 5g tetramethylammonium hydroxide and tetrabutyl hydrogen-oxygen in the autoclave with stirring of 1L Change ammonium mixture (mixture quality ratio is 1:3), airtight test is carried out to reaction kettle, to not occur pressure in reaction kettle 1h Nitrogen displacement and vacuum pumping are carried out to it under the conditions of 50 DEG C after phenomenon, it is ensured that the pumpdown time is greater than 30min, High Purity Nitrogen Then gas displacement number of operations 5 times, row pressure to 0~30KPa are passed through ethylene oxide into reaction kettle, control reaction temperature is 85 DEG C ± 3 DEG C and reaction pressure are 0.3MPa~0.5MPa, until the total amount for being passed through ethylene oxide stops being passed through epoxy when being 10mol Ethane carries out post-processing aging to maintain temperature of reaction kettle being 85 DEG C ± 3 DEG C to product, until reactor pressure no longer declines, table Bright completion slaking reaction.60 DEG C are down to, is neutralized with glacial acetic acid and takes off low boiling.
Prepared propine alcohol ethoxylates are used as nickel plating brightener, then measure the plating piece performance of product and right Than selecting optimal case.
Embodiment 7
The propilolic alcohol of addition 5mol and 5g tetrapropylammonium hydroxide and tetrabutyl hydrogen-oxygen in the autoclave with stirring of 1L Change ammonium mixture (mixture quality ratio is 1:3), airtight test is carried out to reaction kettle, to not occur pressure in reaction kettle 1h Nitrogen displacement and vacuum pumping are carried out to it under the conditions of 50 DEG C after phenomenon, it is ensured that the pumpdown time is greater than 30min, High Purity Nitrogen Then gas displacement number of operations 5 times, row pressure to 0~30KPa are passed through ethylene oxide into reaction kettle, control reaction temperature is 85 DEG C ± 3 DEG C and reaction pressure are 0.3MPa~0.5MPa, until the total amount for being passed through ethylene oxide stops being passed through epoxy when being 10mol Ethane carries out post-processing aging to maintain temperature of reaction kettle being 85 DEG C ± 3 DEG C to product, until reactor pressure no longer declines, table Bright completion slaking reaction.60 DEG C are down to, is neutralized with glacial acetic acid and takes off low boiling.
Prepared propine alcohol ethoxylates are used as nickel plating brightener, then measure the plating piece performance of product and right Than selecting optimal case.
Embodiment 8
The propilolic alcohol of addition 5mol and 5g tetramethylammonium hydroxide and tetrabutyl hydrogen-oxygen in the autoclave with stirring of 1L Change ammonium mixture (mixture quality ratio is 1:3), airtight test is carried out to reaction kettle, to not occur pressure in reaction kettle 1h Nitrogen displacement and vacuum pumping are carried out to it under the conditions of 50 DEG C after phenomenon, it is ensured that the pumpdown time is greater than 30min, High Purity Nitrogen Then gas displacement number of operations 5 times, row pressure to 0~30KPa are passed through ethylene oxide into reaction kettle, control reaction temperature is 85 DEG C ± 3 DEG C and reaction pressure are 0.3MPa~0.5MPa, until the total amount for being passed through ethylene oxide stops being passed through epoxy when being 10mol Ethane carries out post-processing aging to maintain temperature of reaction kettle being 85 DEG C ± 3 DEG C to product, until reactor pressure no longer declines, table Bright completion slaking reaction.60 DEG C are down to, is neutralized with glacial acetic acid and takes off low boiling.
Prepared propine alcohol ethoxylates are used as nickel plating brightener, then measure the plating piece performance of product and right Than selecting optimal case.
Embodiment 9
250~300g/L of nickel sulfate, 50~60g/L of nickel chloride, 40~50g/L of boric acid basal liquid in, be added saccharin 1~2g/L of sodium adds 0.01~0.03g/L of propine alcohol ethoxylate prepared by embodiment 6, at 50~60 DEG C, cathode 3~5A/dm of current density2Under be electroplated.As shown in Figure 1, compared to for old technique, technique of the invention obtains gained nickel coating The nickel coating arrived is more soft, and dispersibility is more preferable, and ray velocity is faster out, it is only necessary to which 3~5min, bright range is wider, bright Agent is more resistant to consumption, and nickel consumption is few, high yield rate;It is integrally full to plate piece, no plating leakage, plating piece the right is the low area of electric current, still full.It is real Apply example 10
Nickel sulfate 250g/L, nickel chloride 50g/L, boric acid 45g/L basal liquid in, be added saccharin sodium 1g/L, add Propine alcohol ethoxylate 0.03g/L prepared by embodiment 6, at 50~60 DEG C, 3~5A/dm of cathode-current density2Lower progress 2A 5min is electroplated, 2A 10min, 2A 10min finally adds the synthesized propine alcohol ethoxylates of the half of initial additive amount Object is closed, continues that 2A 5min is electroplated.Gained nickel coating is as shown in Fig. 2, compared to the plating that for old technique, technique of the invention is obtained Nickel layer is more soft, and dispersibility is more preferable, and ray velocity is faster out, it is only necessary to 3~5min, bright range is wider, brightener more resistant to Consumption, nickel consumption is few, high yield rate.
Fig. 3 is from top to bottom successively are as follows: has used the embodiment of the present invention 6 (the optimal synthetic schemes filtered out) and embodiment 10 The plating piece result that combines combines for plating piece result, old technique that old technique is combined with embodiment 9 with embodiment 10 Propine alcohol ethoxylates plating prepared by plating piece result, the plating piece result combined for product on the market with embodiment 10 The schematic diagram of piece.By comparison, it was found that having used prepared propine alcohol ethoxylate of the invention and using of the present invention The coating that method of coating obtains, effect are best.The bound of each raw material cited by the present invention and each raw material of the present invention, area Between value and bound, the section value of technological parameter (such as temperature, time) can realize the present invention, herein not one by one Enumerate embodiment.
The above is a preferred embodiment of the present invention, cannot limit the right model of the present invention with this certainly It encloses, it is noted that for those skilled in the art, without departing from the principle of the present invention, may be used also To make several improvement and variation, these, which improve and change, is also considered as protection scope of the present invention.

Claims (7)

1. an a kind of one step preparation method of propine alcohol ethoxylates, it is characterised in that: propilolic alcohol and quaternary ammonium bases to be catalyzed Agent is added in reaction kettle, carries out multiple nitrogen displacement and vacuumizes, and then passes to ethylene oxide, and control reaction temperature is 82~88 DEG C, reaction pressure is 0.3MPa~0.5MPa, finally carries out post-processing aging to product, aforesaid reaction vessel temperature is maintained, until Reactor pressure no longer declines, and is down to and is neutralized after 60 DEG C with glacial acetic acid and take off low boiling.
2. an one step preparation method of propine alcohol ethoxylates as described in claim 1, it is characterised in that: the quaternary ammonium base Class catalyst includes tetramethylammonium hydroxide, tetraethyl ammonium hydroxide, tetrapropylammonium hydroxide, one in tetrabutylammonium hydroxide Kind is several.
3. an one step preparation method of propine alcohol ethoxylates as described in claim 1, it is characterised in that: the quaternary ammonium base The additive amount of class catalyst is the 0.05~2% of gross mass.
4. an one step preparation method of propine alcohol ethoxylates as described in claim 1, it is characterised in that: the addition The mole of ethylene oxide is 10mol.
5. an one step preparation method of propine alcohol ethoxylates as described in claim 1, it is characterised in that: the nitrogen is set It changes and vacuum carries out under the conditions of 50 DEG C, the pumpdown time is greater than 30min, and high pure nitrogen is replaced 5 times, row pressure to 0~ 30KPa。
6. an one step preparation method of propine alcohol ethoxylates as described in claim 1, it is characterised in that: the epoxy second Alkane adduct number is 0.5~6mol.
7. a kind of application of propine alcohol ethoxylates as described in claim 1, it is characterised in that: the propilolic alcohol ethoxy Based compound is used as nickel plating brightener, specifically used method are as follows: in 250~300g/L of nickel sulfate, 50~60g/L of nickel chloride, boron In the basal liquid of 40~50g/L of acid, 1~2g/L of saccharin sodium is added, adds propine 0.01~0.03g/L of alcohol ethoxylate, At 50~60 DEG C, 3~5A/dm of cathode-current density2Under be electroplated.
CN201810961349.XA 2018-08-22 2018-08-22 A kind of one one step preparation method of propine alcohol ethoxylates and its application Pending CN109183089A (en)

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CN111620765A (en) * 2020-04-30 2020-09-04 佳化化学(茂名)有限公司 Propiolic alcohol propoxy compound and preparation method thereof
CN114106854A (en) * 2021-11-26 2022-03-01 江苏钟山新材料有限公司 Modified organic silicon surfactant and application thereof

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Application publication date: 20190111