CN103725133A - Preparation method of workshop primer - Google Patents

Preparation method of workshop primer Download PDF

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Publication number
CN103725133A
CN103725133A CN201310695594.8A CN201310695594A CN103725133A CN 103725133 A CN103725133 A CN 103725133A CN 201310695594 A CN201310695594 A CN 201310695594A CN 103725133 A CN103725133 A CN 103725133A
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preparation
dehydrated alcohol
dropping
host
solidifying agent
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CN103725133B (en
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于涛
秦瑞
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Tianjin Meishibang Paint and Chemicals Co Ltd
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Tianjin Meishibang Paint and Chemicals Co Ltd
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Abstract

The invention provides a preparation method of a workshop primer, which comprises the reaction step of carrying out mixing preparation on a main agent and a curing agent according to a weight ratio of 2:1, wherein the preparation of the curing agent comprises the following steps: step 1: sequentially adding two types of reaction liquid of ethyl silicate and absolute ethyl alcohol into a reaction kettle and stirring for 5 to 10min to obtain mixed liquid; step 2: sequentially adding distilled water, 2N hydrochloric acid and absolute ethyl alcohol into a dropping tank of a liquid dropping device to carry out premixing, setting a flow controller in the liquid dropping device and controlling the premixed solution in the dropping device to be added into the mixed liquid in the reaction kettle at a uniform speed within 60-90min; step 3: sequentially adding heavy aromatics, absolute ethyl alcohol, glycol ether and ferric trichloride into the reaction kettle in the step 2 and stirring for 5 to 10min to obtain a curing agent solution. The workshop primer prepared by using the method provided by the invention has excellent adhesion strength and high-temperature resistance after a film is formed by paint, has high film quality, strong weather resistance and excellent corrosion resistance and is low in use cost.

Description

A kind of preparation method of shop primer
Technical field
The invention belongs to technical field of coatings, especially relate to a kind of preparation method of shop primer.
Background technology
Shop primer is the first paint of brushing after surface of steel plate is processed, and also can be called pre-treatment priming paint or maintenance priming paint, mainly for protection steel plate is subject to less atomospheric corrosion in the courses of processing such as welding, cutting, firer's correction.Shop primer is one of important kind of marine finish, and when China's shipbuilding and shipping-trade develop rapidly, the market of shop primer is very broad.Other also need the steel plate pre-treatment of machining large steel construction as bridge, oceanographic engineering etc. in addition, and they also have very large demand to shop primer.Successive dynasties product has zinc wash primer, epoxy zinc-rich paint, epoxy iron oxide red shop primer, inorganic primer for zinc silicate shop.Wherein inorganic zinc silicate primer is mainly to apply kind, mostly be that alcohol dissolubility is from consolidating type, generally formulated by coating host and solidifying agent, in host, mainly with zinc powder, be main rust-stabilising pigment, form zinc silicate, iron composite salt with solidifying agent hybrid reaction and close attachment in steel surface.After the effect of solidifying agent is oil paint coating, can continues hydrolytic polymerization and become caking agent, play bonding effect, what mostly adopt at present is the major ingredient of silicate hydrolyzate liquid as solidifying agent.Silicate hydrolyzate liquid is as filmogen, plays bonding effect, select suitable degree of hydrolysis after hydrolysate film forming good, just can there is excellent adhesion strength and high-temperature behavior.Therefore the selection of solidifying agent has great impact to the performance of shop primer.
At present, specification of quality for shop primer is: the approximately 20 μ left and right individual layer paint films that general requirement applies on steel plate, at its antirust ability in marine atmosphere or industrial atmosphere, at least should there be 3 months, there is good shock-resistant and toughness simultaneously, less and there is hypotoxicity in welding, cutting and firer's timing paint film heat-affected zone, especially should not produce too much harmful poison gas etc. during paint film decomposes.And at present poor heat stability, weathering resistance deficiency in use often appear in shop primer on the market, the phenomenon such as unstable after coating film forming, has affected the antiseptic property of coating greatly.Especially to oil carrier, in offshore oil platform, to the large-scale steel and iron member pre-treatment primary coat used time, above-mentioned situation is more common, and the antiseptic property of coating is poor very large to the infringement of steel construction piece.
Summary of the invention
For solving the problems of the technologies described above, the invention provides a kind of good weatherability, anticorrosion working life long shop primer preparation method, while being particularly useful in the environment such as oil carrier, offshore oil platform large-scale steel and iron member pre-treatment primary coat, use.
The invention provides a kind of preparation method of shop primer, comprise following reactions steps:
With host and solidifying agent 2:1 mixed preparing by weight, wherein the preparation process of solidifying agent is:
Step 1: tetraethyl silicate, two kinds of reaction solutions of dehydrated alcohol are added in reactor successively, stir 5-10min and obtain mixed solution;
Step 2: distilled water, 2N hydrochloric acid, dehydrated alcohol are added successively in the dropping liquid tank of fluid drips feeder apparatus and carry out pre-mixing, set the flow director in fluid drips feeder apparatus, the aqueous premix of controlling in Dropping feeder is at the uniform velocity added in the mixed solution in reactor in 60-90min;
Step 3: add successively heavy aromatics, dehydrated alcohol, ethylene glycol ethyl ether, iron trichloride in the reactor in step 2, stir 5-10min, obtain curing agent solution.
Wherein tetraethyl silicate silicon content is 40 ± 2%; Described heavy aromatics is heavy aromatics p-4.
In the preparation process of above-mentioned solidifying agent, in step 2, be also included in distilled water, 2N hydrochloric acid, dehydrated alcohol and add successively in dropping liquid tank after pre-mixing, start to be added dropwise to before reactor, set in advance the lower position that in dropping liquid tank, liquid level control sensor test liquid level declines; After dropping starts, the liquid level of aqueous premix drops to default lower position, and liquid level control sensor starts to send sound and light alarm, remind operating personnel's step 2 to complete, should enter rapidly next step, prevent from reacting the break period long, affect the quality of final curing agent solution.
Further above-mentioned preparation method, also comprises host preparation process:
Grind: by acid polyethylene butyraldehyde liquid, white carbon black, wilkinite GBP-183, titanium dioxide NTR-606, compound ferrophosphorus powder, silica powder 350 orders, industrial alcohol, dimethylbenzene mixed grinding, obtain grinding product;
Be in harmonious proportion: in grinding product, add successively zinc powder, anti-sagging agent 3300X, through high speed shear, be uniformly dispersed, be deployed into host.
The component adding in the preparation process of above-mentioned host is respectively:
Figure BDA0000435622450000021
Figure BDA0000435622450000031
The component adding in the preparation process of solidifying agent is respectively: the tetraethyl silicate adding in step 1 is 25-40 part, dehydrated alcohol 5-10 part; Distilled water 5-10 part, 2N hydrochloric acid 0.3-0.8 part, dehydrated alcohol 10-15 part in step 2; Heavy aromatics 1-10 part, dehydrated alcohol 15-25 part, ethylene glycol ethyl ether 2-10 part, iron trichloride 0.1-0.8 part in step 3.
When coating host is mainly used for antiseptic and rustproof and high-temperature heating, form firm coating.In the preparation of host, acid polyethylene butyraldehyde liquid is membrane-forming agent, also makes moulding paint film have good toughness; Wilkinite GBP-183 and silica powder 350 orders are anti-settling agent; White carbon black is called again precipitated silica, is the toughner of welding iron and steel; Compound ferrophosphorus powder is a kind of heat-resisting and good rust-stabilising pigment of conductivity, can partly replace high zinc powder simultaneously, reduces the use of zinc powder, reduces costs; Titanium dioxide can reduce zinc powder atomization when welding; Industrial alcohol and dimethylbenzene are solvent, and adding of alcoholic solvent is the polarity in order to change solvent, promote opening and disperseing of anti-settling agent, pigment, filler; Zinc powder is main rust protection material.
In the preparation of shop primer, silicate hydrolyzate liquid is as filmogen, plays bonding effect, only have select suitable degree of hydrolysis after hydrolysate film forming good, just can have excellent adhesion strength and high-temperature behavior, be also that the selection of solidifying agent in shop primer is huge to the performance impact of shop primer.
Solidifying agent preparation principle is under catalyst action, to allow the product of tetraethyl silicate hydrolytic polymerization formation in advance macromolecular chain, then after mixing with coating host, forms macromolecular reticulated structure, i.e. paint film coating.In the preparation method of solidifying agent of the present invention, tetraethyl silicate is polymerization adhesives, and dehydrated alcohol and Virahol are thinners, and iron trichloride and 2N hydrochloric acid are catalyzer, promotes hydrolysis and the polymerization of tetraethyl silicate, and distilled water is for hydrolysis and the polyreaction of tetraethyl silicate; Heavy aromatics p-4 is the solvent as tetraethyl silicate, is the commercially available prod of Tianjin Tong Xuan chemical company.
In general solidifying agent preparation method, be first hydrochloric acid, dehydrated alcohol, distilled water to be mixed and is added drop-wise in tetraethyl silicate, then add heavy aromatics, ethylene glycol ethyl ether, dehydrated alcohol, iron trichloride.The reaction of shop primer liquid is thermopositive reaction, and the control of reaction soln rate of addition is bad, can make reacted molecular size inhomogeneous, makes after coating film forming unstablely, affects antiseptic property.Therefore keep the even velocity of flow of dropping very important, in addition because the time dripping is in 60-90min, in production, used flow director to replace manual operation, saved human cost; In dropping liquid tank, add and put liquid level control sensor simultaneously, when liquid level arrives lower position in dropping liquid tank, send sound and light alarm, remind operating personnel to enter rapidly step 3, guaranteed that the success of solidifying agent preparation feedback is carried out, improve preparation efficiency and yield simultaneously, greatly reduced cost of labor.
In the present invention in the preparation process of solidifying agent, step 1 first joins dehydrated alcohol in tetraethyl silicate, because also there is dehydrated alcohol tetraethyl silicate the inside, dropping solution in step 2 can be merged with mixed solution better, impel reaction to carry out smoothly, reacted molecular size is more uniform and stable.Meanwhile, the reaction of solidifying agent is thermopositive reaction, and the rate of addition of therefore controlling well is the key point of this technique, is also the key of controlling this product quality and stability.In the present invention, contriver gropes by long test, while finding the rate of addition in step 2 or time to be controlled at 60min-90min, can improve bulk of molecule uniformity coefficient after solidifying agent reaction.
In addition, after the solidifying agent obtaining mixes with coating, accelerate speed of response through prehydrolysis and polymerization, selected again dehydrated alcohol that volatility is good as diluting solvent simultaneously, made coating can complete rapidly surface drying after spraying.
The shop primer that uses the inventive method to prepare, after coating film forming, there is excellent adhesion strength, resistance to elevated temperatures, film quality is good, weathering resistance is strong, antiseptic property excellence, use cost is low, while being particularly useful in the environment such as oil carrier, offshore oil platform large-scale steel and iron member pre-treatment primary coat, uses.
Embodiment
Below in conjunction with embodiment, the invention will be further described, but can not serve as restriction of the present invention.
A preparation method for shop primer, is comprised of following reactions steps preparation:
1) host preparation process:
Grind: by acid polyethylene butyraldehyde liquid, white carbon black, wilkinite GBP-183, titanium dioxide NTR-606, compound ferrophosphorus powder, silica powder 350 orders, industrial alcohol, dimethylbenzene mixed grinding, obtain grinding product;
Be in harmonious proportion: in grinding product, add successively zinc powder, anti-sagging agent 3300X, through high speed shear, be uniformly dispersed, be deployed into host;
2) preparation process of solidifying agent is:
Step 1: tetraethyl silicate, two kinds of reaction solutions of dehydrated alcohol are added in reactor successively, stir 5min and obtain mixed solution;
Step 2: distilled water, 2N hydrochloric acid, dehydrated alcohol are added successively in the dropping liquid tank of fluid drips feeder apparatus and carry out pre-mixing, set the flow director in fluid drips feeder apparatus, the aqueous premix of controlling in Dropping feeder is at the uniform velocity added in the mixed solution in reactor in 60min; Before dropping, set in advance the lower position that in dropping liquid tank, liquid level control sensor test liquid level declines simultaneously; After dropping starts, the liquid level of aqueous premix drops to default lower position, and liquid level control sensor starts to send sound and light alarm, reminds operating personnel's step 2 to complete, and should enter rapidly step 3;
Step 3: add successively heavy aromatics, dehydrated alcohol, ethylene glycol ethyl ether, iron trichloride in the reactor in step 2, stir 10min, obtain curing agent solution.
3) host, solidifying agent are in harmonious proportion step: by prepare gained host and curing agent solution by weight 2:1 ratio mix, obtain described highly corrosion resistant shop primer.
In above-mentioned host preparation process, the addition of each component is:
Figure BDA0000435622450000051
About the interpolation of dehydrated alcohol, in step 1, the addition of dehydrated alcohol is 50kg; In step 2, the addition of dehydrated alcohol is 100kg; In step 3, the addition of dehydrated alcohol is 150kg.
Wherein above-mentioned tetraethyl silicate silicon content is 40 ± 2%.
Embodiment 2:
A preparation method for shop primer, is comprised of following reactions steps preparation:
1) host preparation process:
Grind: by acid polyethylene butyraldehyde liquid, white carbon black, wilkinite GBP-183, titanium dioxide NTR-606, compound ferrophosphorus powder, silica powder 350 orders, industrial alcohol, dimethylbenzene mixed grinding, obtain grinding product;
Be in harmonious proportion: in grinding product, add successively zinc powder, anti-sagging agent 3300X, through high speed shear, be uniformly dispersed, be deployed into host;
2) preparation process of solidifying agent is:
Step 1: tetraethyl silicate, two kinds of reaction solutions of dehydrated alcohol are added in reactor successively, stir 10min and obtain mixed solution;
Step 2: distilled water, 2N hydrochloric acid, dehydrated alcohol are added successively in the dropping liquid tank of fluid drips feeder apparatus and carry out pre-mixing, set the flow director in fluid drips feeder apparatus, the aqueous premix of controlling in Dropping feeder is at the uniform velocity added in the mixed solution in reactor in 90min; Before dropping, set in advance the lower position that in dropping liquid tank, liquid level control sensor test liquid level declines simultaneously; After dropping starts, the liquid level of aqueous premix drops to default lower position, and liquid level control sensor starts to send sound and light alarm, reminds operating personnel's step 2 to complete, and should enter rapidly step 3;
Step 3: add successively heavy aromatics, dehydrated alcohol, ethylene glycol ethyl ether, iron trichloride in the reactor in step 2, stir 10min, obtain curing agent solution.
3) host, solidifying agent are in harmonious proportion step: by prepare gained host and curing agent solution by weight 2:1 ratio mix, obtain described highly corrosion resistant shop primer.
In above-mentioned host preparation process, the addition of each component is:
Figure BDA0000435622450000061
In above-mentioned solidifying agent preparation process, the interpolation of each component is as follows:
Figure BDA0000435622450000071
About the interpolation of dehydrated alcohol, in step 1, the addition of dehydrated alcohol is 100kg; In step 2, the addition of dehydrated alcohol is 150kg; In step 3, the addition of dehydrated alcohol is 250kg;
Wherein above-mentioned tetraethyl silicate silicon content is 40 ± 2%.
Embodiment 3:
A preparation method for shop primer, is comprised of following reactions steps preparation:
1) host preparation process:
Grind: by acid polyethylene butyraldehyde liquid, white carbon black, wilkinite GBP-183, titanium dioxide NTR-606, compound ferrophosphorus powder, silica powder 350 orders, industrial alcohol, dimethylbenzene mixed grinding, obtain grinding product;
Be in harmonious proportion: in grinding product, add successively zinc powder, anti-sagging agent 3300X, through high speed shear, be uniformly dispersed, be deployed into host;
2) preparation process of solidifying agent is:
Step 1: tetraethyl silicate, two kinds of reaction solutions of dehydrated alcohol are added in reactor successively, stir 5min and obtain mixed solution;
Step 2: distilled water, 2N hydrochloric acid, dehydrated alcohol are added successively in the dropping liquid tank of fluid drips feeder apparatus and carry out pre-mixing, set the flow director in fluid drips feeder apparatus, the aqueous premix of controlling in Dropping feeder is at the uniform velocity added in the mixed solution in reactor in 90min; Before dropping, set in advance the lower position that in dropping liquid tank, liquid level control sensor test liquid level declines simultaneously; After dropping starts, the liquid level of aqueous premix drops to default lower position, and liquid level control sensor starts to send sound and light alarm, reminds operating personnel's step 2 to complete, and should enter rapidly step 3;
Step 3: add successively heavy aromatics, dehydrated alcohol, ethylene glycol ethyl ether, iron trichloride in the reactor in step 2, stir 10min, obtain curing agent solution.
3) host, solidifying agent are in harmonious proportion step: by prepare gained host and curing agent solution by weight 2:1 ratio mix, obtain described highly corrosion resistant shop primer.
In above-mentioned host preparation process, the addition of each component is:
In above-mentioned solidifying agent preparation process, the interpolation of each component is as follows:
Figure BDA0000435622450000082
About the interpolation of dehydrated alcohol, in step 1, the addition of dehydrated alcohol is 60kg; In step 2, the addition of dehydrated alcohol is 150kg; In step 3, the addition of dehydrated alcohol is 190kg;
Wherein, above-mentioned tetraethyl silicate silicon content is 40 ± 2%.
The product being made by the preparation method described in embodiment 1-3 and commercially available shop primer are contrasted, and actual detection data are as follows:
Figure BDA0000435622450000083
Figure BDA0000435622450000091
By above-mentioned test data, can be seen and be adopted the shop primer prepared of the inventive method, sticking power is stronger, surface drying time is fast, and weathering resistance is high, and in salt fog resistance, the environment such as be exposed to the sun, paint film property is more excellent.
Treatment process of the present invention is described by specific embodiment.Those skilled in the art can use for reference the links such as content appropriate change raw material of the present invention, processing condition and realize corresponding other object, its relevant change does not all depart from content of the present invention, all similar replacements and change apparent to those skilled in the art, within being all deemed to be included in scope of the present invention.

Claims (7)

1. a preparation method for shop primer, is characterized in that comprising following reactions steps:
With host and solidifying agent 2:1 mixed preparing by weight, wherein the preparation process of solidifying agent is:
Step 1: tetraethyl silicate, two kinds of reaction solutions of dehydrated alcohol are added in reactor successively, stir 5-10min and obtain mixed solution;
Step 2: distilled water, 2N hydrochloric acid, dehydrated alcohol are added successively in the dropping liquid tank of fluid drips feeder apparatus and carry out pre-mixing, set the flow director in fluid drips feeder apparatus, the aqueous premix of controlling in Dropping feeder is at the uniform velocity added in the mixed solution in reactor in 60-90min;
Step 3: add successively heavy aromatics, dehydrated alcohol, ethylene glycol ethyl ether, iron trichloride in the reactor in step 2, stir 5-10min, obtain curing agent solution.
2. preparation method according to claim 1, characterized by further comprising host preparation process:
Grind: by acid polyethylene butyraldehyde liquid, white carbon black, wilkinite GBP-183, titanium dioxide NTR-606, compound ferrophosphorus powder, silica powder 350 orders, industrial alcohol, dimethylbenzene mixed grinding, obtain grinding product;
Be in harmonious proportion: in grinding product, add successively zinc powder, anti-sagging agent 3300X, through high speed shear, be uniformly dispersed, be deployed into host.
3. preparation method according to claim 1, is characterized in that described tetraethyl silicate silicon content is 40 ± 2%.
4. preparation method according to claim 1, is characterized in that described heavy aromatics is heavy aromatics p-4.
5. preparation method according to claim 1, it is characterized in that in the preparation process of solidifying agent, in step 2, be also included in distilled water, 2N hydrochloric acid, dehydrated alcohol and add successively in dropping liquid tank after pre-mixing, start to be added dropwise to before reactor, set in advance the lower position that in dropping liquid tank, liquid level control sensor test liquid level declines; After dropping starts, the liquid level of aqueous premix drops to default lower position, and liquid level control sensor starts to send sound and light alarm.
6. preparation method according to claim 2, is characterized in that counting by weight, and the component adding in the preparation process of host is respectively:
Figure FDA0000435622440000011
Figure FDA0000435622440000021
7. according to the preparation method described in claim 1-6 any one, it is characterized in that counting by weight, the component adding in the preparation process of solidifying agent is respectively: the tetraethyl silicate adding in step 1 is 25-40 part, dehydrated alcohol 5-10 part; Distilled water 5-10 part, 2N hydrochloric acid 0.3-0.8 part, dehydrated alcohol 10-15 part in step 2; Heavy aromatics 1-10 part, dehydrated alcohol 15-25 part, ethylene glycol ethyl ether 2-10 part, iron trichloride 0.1-0.8 part in step 3.
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