CN107815162A - A kind of alcamines multifunctional assistant and preparation method and application - Google Patents

A kind of alcamines multifunctional assistant and preparation method and application Download PDF

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Publication number
CN107815162A
CN107815162A CN201710855300.1A CN201710855300A CN107815162A CN 107815162 A CN107815162 A CN 107815162A CN 201710855300 A CN201710855300 A CN 201710855300A CN 107815162 A CN107815162 A CN 107815162A
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Prior art keywords
alcamines
multifunctional assistant
preparation
room temperature
parts
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CN201710855300.1A
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CN107815162B (en
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丁贤勇
张胜
王振兴
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GUANGZHOU LEOBO PAINT SCIENCE & TECHNOLOGY Co Ltd
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GUANGZHOU LEOBO PAINT SCIENCE & TECHNOLOGY Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/14Paints containing biocides, e.g. fungicides, insecticides or pesticides
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C213/00Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C213/00Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton
    • C07C213/08Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton by reactions not involving the formation of amino groups, hydroxy groups or etherified or esterified hydroxy groups

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Plant Pathology (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Paints Or Removers (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The invention discloses a kind of alcamines multifunctional assistant and preparation method and application, the preparation method of the alcamines multifunctional assistant comprises the following steps:S1,120 150 parts of diethanol amine are placed in container, 30 45 parts of paraformaldehydes that addition while stirring has been dissolved with solvent at room temperature, react 0.5 1h;S2, addition 0.5 1 parts of catalyst and 30 50 parts of hydrochloric acid into container, react 12 hours at room temperature, and then plus water stirs 10 30 minutes, obtains clear viscous alcamines multifunctional assistant.Alcamines multifunctional assistant prepared by the present invention can be used as pH value regulator, and the dosage of dispersant can be substantially reduced while own smell is reduced, have the function that bactericidal can be used as antiseptic simultaneously, avoid the performance that excessive promoter effect paint film is added in coating, and itself can slowly volatilization be walked from paint film, so as to improve the glossiness of paint film.

Description

A kind of alcamines multifunctional assistant and preparation method and application
Technical field
The present invention relates to coating additive field, and more specifically, the present invention relates to a kind of alcamines multifunctional assistant and its system Preparation Method and application.
Background technology
Coating is mainly by film forming matter, pigment, filler and various auxiliary agents composition.Auxiliary agent includes thickener, defoamer, profit Humectant, dispersant, levelling agent, anticorrosion and bactericidal agent etc., wherein, pH value conditioning agent not only plays the work of pH value regulation in coating With, pigment can also be disperseed, make coating system stable, and do not flocculated during storage, dispersant can be substantially reduced Dosage, beneficial to the performance for improving coating paint film.At present, the pH value regulator in market mainly has AMP-95, AMP-90, ammoniacal liquor, burns Alkali, N- methylethanolamines, dimethylethanolamine etc., except ammoniacal liquor, outside dimethylethanolamine, their boiling point all more than 150 DEG C, Boiling point is higher, and volatilization is slower, and smell is lower, and the value of environmental protection is higher.Now coating with widest pH value conditioning agent is AMP- 95 conditioning agents, there is an alcoholic extract hydroxyl group in its structure, alcoholic extract hydroxyl group, which can adsorb inorganic pigment, makes its surface positively charged, in electrostatic interaction Lower solution flocks, are stably dispersed in coating system.But AMP-95 ammoniacal liquor taste is heavier, bad with the compatibility of anticorrosion and bactericidal agent.
The content of the invention
Based on this, the defects of the invention reside in prior art is overcome, there is provided a kind of alcamines multifunctional assistant, the hydramine Class multifunctional assistant can be used as pH value regulator, and the use of dispersant can be substantially reduced while own smell is reduced Amount, while there is bactericidal, antiseptic can be used as, avoids and excessive promoter effect paint film is added in coating Performance, and itself can slowly volatilization be walked from paint film, so as to improve the glossiness of paint film.
Its technical scheme is as follows:
A kind of alcamines multifunctional assistant, structure are as shown in Equation 1:
Alcamines multifunctional assistant of the present invention is similar with pH adjusting agent AMP-95 structures, has the regulation of preferable pH value Effect, can be used as pH adjusting agent;The alcamines multifunctional assistant contains 2 alcoholic extract hydroxyl groups, substantially increases to inorganic pigment Suction-operated, its surface is become positively charged lotus, inorganic pigment solution flocks, uniform and stable point can be made in the presence of electrostatic repulsion It is dispersed in coating system;Multifunctional assistant molecular weight is 153.5, and structure is bigger than AMP-95 in umbrella, therefore steric hindrance acts on It is bigger than AMP-95, the reunion of inorganic pigment can be prevented under steric hindrance effect;The multifunctional assistant introduces Cl, has Bactericidal bacteriostasis.
The preparation method of the alcamines multifunctional assistant, comprises the following steps:
S1,120-150 part diethanol amine is placed in container, addition while stirring at room temperature has been dissolved with solvent 30-45 part paraformaldehydes, react 0.5-1h;
S2, added into container and use 0.5-1 parts catalyst and 30-50 part hydrochloric acid, react 1-2 hour at room temperature, so Afterwards plus water stirs 10-30 minutes, obtains clear viscous alcamines multifunctional assistant.
Its synthetic route is as follows:
In one of the embodiments, the step S1 is:It is in liquid that diethanol amine is put into 90 DEG C of bakingizations in baking oven, Then 120-150 part diethanol amine is placed in three-necked flask, at room temperature mechanical agitation, adds isopropanol dissolving while stirring Good 30-45g paraformaldehydes, react 0.5-1h.
In one of the embodiments, catalyst described in step S2 is sodium borohydride.
Application of the alcamines multifunctional assistant as pH adjusting agent among coating system.
Application of the alcamines multifunctional assistant as bactericide among coating system.
In one of the embodiments, the coating system is water-proof acrylic acid paint system.
The beneficial effects of the present invention are:The present invention is prepared for a kind of alcamines multifunctional assistant, the more work(of alcamines Energy auxiliary agent is similar with pH adjusting agent AMP-95 structures, has preferable pH adjustment effects;Compared to AMP-95, the alcamines is more The more alcoholic extract hydroxyl groups of function additive, substantially increase the suction-operated to inorganic pigment, its surface is become positively charged lotus, quiet Inorganic pigment solution flocks can be made in the presence of electric repulsion, and its structure is in umbrella, it is bigger than AMP-95, therefore steric hindrance effect ratio AMP-95 is big, and the reunion of inorganic pigment can be prevented under steric hindrance effect, make inorganic pigment it is uniform and stable be dispersed in painting In material system;Alcamines multifunctional assistant of the present invention contains Cl, has bactericidal bacteriostasis, can be applied to as antiseptic In coating system;The preparation method that the present invention prepares the alcamines multifunctional assistant is simple, and time-consuming short, reaction stability is good, Low raw-material cost, suitable for commercial Application.
Brief description of the drawings
Fig. 1 is the infrared spectrogram of alcamines multifunctional assistant described in embodiment 1.
Embodiment
For the objects, technical solutions and advantages of the present invention are more clearly understood, below in conjunction with accompanying drawing and specific embodiment party Formula, the present invention is described in further detail.It should be appreciated that embodiment described herein is only solving The present invention is released, does not limit protection scope of the present invention.
Embodiment 1
A kind of alcamines multifunctional assistant, is prepared as follows:
S1, diethanol amine is put into 90 DEG C of bakingizations in baking oven is in liquid, and 140 parts of diethanol amine then are placed in into three mouthfuls of burnings In bottle, mechanical agitation, adds 40 parts of paraformaldehydes that isopropanol has dissolved while stirring at room temperature, reacts 0.5h.
S2, added into three-necked flask with 0.6 part of catalyst sodium borohydride and 40 parts of hydrochloric acid, at room temperature reaction 1.5 Hour, then plus deionized water stirs 20 minutes, obtains clear viscous material, that is, obtains alcamines multifunctional assistant.
Synthetic route is as follows:
Gained alcamines multifunctional assistant with the strainer filtering of 250 mesh and then is subjected to infrared test, the infrared figure of test gained See Fig. 1.It was found from figure:3298cm-1For-OH characteristic absorption peak, in 1046cm-1Place has the sharp stronger absworption peak to be C-O stretching vibration peak, C-N stretching vibrations, which absorb, is sewn on 1358cm-1Place, in 1454cm-1There is a weaker and wide absorption at place It is C-H flexural vibrations, 736cm-1There is the characteristic peak that a weaker absworption peak is C-Cl at place.Therefore, can by atlas analysis To judge to have obtained target product alcamines multifunctional assistant.
Embodiment 2
A kind of alcamines multifunctional assistant, as follows:
S1, diethanol amine is put into 90 DEG C of bakingizations in baking oven is in liquid, and 120 parts of diethanol amine then are placed in into three mouthfuls of burnings In bottle, mechanical agitation, adds 30 parts of paraformaldehydes that isopropanol has dissolved while stirring at room temperature, reacts 1h.
S2, addition 0.5 part of catalyst sodium borohydride and 30 parts of hydrochloric acid into three-necked flask, react at room temperature 2 small When, then plus deionized water stirs 10 minutes, obtains clear viscous material.Its character is same as Example 1, shows to have obtained institute State alcamines multifunctional assistant.
Embodiment 3
A kind of alcamines multifunctional assistant, as follows:
S1, diethanol amine is put into 90 DEG C of bakingizations in baking oven is in liquid, and 150 parts of diethanol amine then are placed in into three mouthfuls of burnings In bottle, mechanical agitation, adds 45 parts of paraformaldehydes that isopropanol has dissolved while stirring at room temperature, reacts 0.5h.
S2, addition 1 part of catalyst sodium borohydride and 50 parts of hydrochloric acid into three-necked flask, react 1 hour at room temperature, Then plus deionized water stirs 30 minutes, obtains clear viscous material.Its character is same as Example 1, shows to have obtained described Alcamines multifunctional assistant.
Alcamines multifunctional assistant, AMP-95, the ammoniacal liquor prepared to embodiment 1 carries out performance test, method of testing or mark It is accurate as follows:
(1) boiling point:Using microdetermination boiling point;
(2) viscosity:With DV-C rotation viscometers, determined at 25 DEG C of room temperature;
(3) resistance to blocking:With reference to resistance to blocking testing standard GB/T23982;
(4) pH value/mass fraction 1%:With pH value tester (PHS-3C acid-base meters);
(5) low smell:At room temperature, the beaker equipped with sample, lid is opened, hears size, the excitant of sample smell;
(6) to pigment-dispersing ability:A certain amount of pigment is added into water, is disperseed with small-sized dispersion machine is tested, slowly added Enter experiment prepare multifunctional assistant, after certain time sampling scratched with scraper in art post paperboard, observe art post paperboard on whether have Particle, if without particle, it is good to pigment-dispersing ability to show;If there is particle, the quantity of particle is recorded, par is 1~5/cm2 When, show general to pigment-dispersing ability;More than 5/cm2, it is poor to pigment-dispersing ability to show.
Test result is shown in Table 1.
Table 1
From above AMP-95, alcamines multifunctional assistant, ammoniacal liquor performance comparison, the alcamines for preparing of the present invention is more The low temperature flow of function additive is better than AMP-95, and pH value is lower than AMP-95, and smell is lower than AMP-95, has good ring Support value value, and the stably dispersing of pigment is made good use of, beneficial to the storage of coating.
The alcamines multifunctional assistant of synthesis is added in water-proof acrylic acid emulsion as bactericide, with non-adding of germicide Water-proof acrylic acid emulsion contrasted, observe bacteria breed, comprise the following steps that:By water-proof emulsion and water according to 1:10 ratio Example prepares, and is drawn with suction pipe, then drips 10 and drips among Bacteria Culture paper, be put into dry glass culture dish, sees daily The growth diffusion velocity for examining bacterium (has pore explanation occur to have bacterium appearance, recorded the number of stain in the centre of culture paper Amount).Experimental result is as shown in table 2.
Table 2
Number of days/d 1 3 6 10 15 20 25 30
Alcamines multifunctional assistant/point Nothing Nothing Nothing Nothing Nothing 1 2 5
Non- adding of germicide/point Nothing 2 5 8 16 30 - -
As shown in Table 2, the alcamines multifunctional assistant that prepared by the present invention has good bactericidal bacteriostasis.
Each technical characteristic of embodiment described above can be combined arbitrarily, to make description succinct, not to above-mentioned reality Apply all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited In contradiction, the scope that this specification is recorded all is considered to be.
Embodiment described above only expresses the several embodiments of the present invention, and its description is more specific and detailed, but simultaneously Can not therefore it be construed as limiting the scope of the patent.It should be pointed out that come for one of ordinary skill in the art Say, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the protection of the present invention Scope.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.

Claims (7)

1. a kind of alcamines multifunctional assistant, it is characterised in that structure is as shown in Equation 1:
2. the preparation method of alcamines multifunctional assistant described in claim 1, it is characterised in that comprise the following steps:
S1,120-150 part diethanol amine is placed in container, the 30-45 that addition while stirring has been dissolved with solvent at room temperature Part paraformaldehyde, reacts 0.5-1h;
S2,0.5-1 parts catalyst and 30-50 part hydrochloric acid are added into container, react 1-2 hour at room temperature, then add water Stirring 10~30 minutes, obtains clear viscous alcamines multifunctional assistant.
3. preparation method according to claim 2, it is characterised in that the step S1 is:Diethanol amine is put into baking oven In 90 DEG C of bakingizations be in liquid, then 120-150 part diethanol amine is placed in three-necked flask, at room temperature mechanical agitation, while stirring Mix side and add 30-45 part paraformaldehydes that isopropanol has dissolved, react 0.5-1h.
4. preparation method according to claim 2, it is characterised in that catalyst described in step S2 is sodium borohydride.
5. application of the alcamines multifunctional assistant as pH adjusting agent among coating system described in claim 1.
6. application of the alcamines multifunctional assistant as bactericide among coating system described in claim 1.
7. apply according to claim 6, it is characterised in that the coating system is water-proof acrylic acid paint system.
CN201710855300.1A 2017-09-20 2017-09-20 Multifunctional alcohol amine assistant and preparation method and application thereof Active CN107815162B (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5692909A (en) * 1979-12-26 1981-07-28 Kyoritsu Yuki Kogyo Kenkyusho:Kk Production of water-soluble cationized melamine resin
CN104311403A (en) * 2014-10-08 2015-01-28 中国科学院过程工程研究所 Production method for methylacrolein

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5692909A (en) * 1979-12-26 1981-07-28 Kyoritsu Yuki Kogyo Kenkyusho:Kk Production of water-soluble cationized melamine resin
CN104311403A (en) * 2014-10-08 2015-01-28 中国科学院过程工程研究所 Production method for methylacrolein

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
顾可权: "《重要有机化学反应 第二版》", 31 January 1984, 上海科学技术出版社 *

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