CN109970072B - Water glass pretreatment process - Google Patents
Water glass pretreatment process Download PDFInfo
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- CN109970072B CN109970072B CN201910407668.0A CN201910407668A CN109970072B CN 109970072 B CN109970072 B CN 109970072B CN 201910407668 A CN201910407668 A CN 201910407668A CN 109970072 B CN109970072 B CN 109970072B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/32—Alkali metal silicates
- C01B33/325—After-treatment, e.g. purification or stabilisation of solutions, granulation; Dissolution; Obtaining solid silicate, e.g. from a solution by spray-drying, flashing off water or adding a coagulant
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Abstract
The invention relates to a water glass treatment process, which comprises the following steps: (1) Adding water glass with the modulus of 3.2-3.7 and water into a rotary spherical digester, and sealing; (2) Introducing water vapor into the rotary spherical digester in the step (1) to ensure that the pressure in the rotary spherical digester reaches 0.08-0.15 MPa, and maintaining the pressure for 4-6 hours to obtain a water glass solution; (3) Feeding the water glass solution obtained in the step (2) into a middle-rotating dispersion tank, reducing the temperature to 75-90 ℃, adding a treating agent, and stirring for 20-60 minutes at the rotating speed of 70-110 r/min; the water glass pretreated by the process can be directly reacted with sulfuric acid in the subsequent synthesis process, so that the aim of quick reaction is fulfilled, the time cost in the production process is saved, and the special application effect of the water glass in the terminal product is shown, for example: excellent anti-settling property and excellent dispersibility. And the pretreatment is carried out in the water glass link through the accurate adding proportion, so that the quality stability of the terminal product is higher.
Description
Technical Field
The invention relates to a water glass treatment process, in particular to a water glass pretreatment process.
Background
Water glass is a water-soluble silicate which consists of alkali metal and silica in different proportions. Most commonly used is sodium silicate water glass Na 2 O·nSiO 2 Also potassium silicate K 2 O·nSiO 2 . The molar ratio of silica to sodium oxide (or potassium oxide) in the water glass composition is generally referred to as the modulus M.
The modulus of water glass produced in China is generally between 2.4 and 3.3. The content (or concentration) of water glass in an aqueous solution is often expressed in terms of density or baume. The density of the common water glass in civil engineering is generally 1.36-1.50 g/cm 3 Corresponding to baume of 38.4 to 48.3. The higher the density, the higher the water glass content and the higher the viscosity. The water glass is usually quartz powder (SiO) 2 ) Adding sodium carbonate (Na) 2 CO 3 ) Calcining at 1300-1400 deg.C to generate solid, and dissolving in high-temp or high-temp high-pressure water to obtain the water glass in solution form.
The water glass prepared by the prior art method has poor dispersibility in the use process, is used for influencing the glossiness in the paint, is easy to settle, and influences the use effect.
Disclosure of Invention
Aiming at some problems existing in the prior art, the invention provides a water glass pretreatment process, which comprises the following steps:
(1) Adding water glass with the modulus of 3.2-3.7 and water into a rotary spherical digester, and sealing;
(2) Introducing water vapor into the rotary spherical digester in the step (1) to ensure that the pressure in the rotary spherical digester reaches 0.08-0.15 MPa, and maintaining the pressure for 4-6 hours to obtain a water glass solution;
(3) And (3) feeding the water glass solution obtained in the step (2) into a middle-rotating dispersion tank, reducing the temperature to 75-90 ℃, adding a treating agent, and stirring for 20-60 minutes at the rotating speed of 70-110 r/min.
As a preferable technical scheme of the invention, the mass ratio of the water glass to the water in the step (1) is (1.0-3.0) (1.5-6.0).
As a preferable technical scheme of the invention, the mass ratio of the water glass to the water in the step (1) is (1.0-2.0) to (3.0-5.0).
As a preferable technical scheme of the invention, the pressure in the rotary spherical digester in the step (2) is 0.08-0.1 MPa.
As a preferable technical scheme of the invention, the temperature of the step (3) is reduced to 78-85 ℃.
As a preferable technical scheme of the invention, the treating agent in the step (3) is selected from one or more of oxidized polyethylene wax, oxidized paraffin wax and oxidized microcrystalline wax.
As a preferred embodiment of the present invention, the treating agent in step (3) further comprises an auxiliary agent.
As a preferable technical scheme of the invention, the auxiliary agent is one of nonionic surfactant alkylphenol ethoxylates or nonionic surfactant fatty alcohol polyoxyethylene ethers.
As a more preferable technical scheme of the invention, the auxiliary agent is alkylphenol ethoxylate.
As a preferable technical scheme of the invention, the alkylphenol ethoxylates are selected from one or more of nonylphenol ethoxylates, pentylphenol ethoxylates, octylphenol ethoxylates, decylphenol ethoxylates, undecylphenol ethoxylates, dodecylphenol ethoxylates and pentadecylphenol ethoxylates.
Compared with the prior art, the invention has the following advantages: the water glass pretreated by the process can be directly reacted with sulfuric acid in the subsequent synthesis process, so that the aim of quick reaction is fulfilled, the time cost in the production process is saved, and the special application effect of the water glass in the terminal product is shown, for example: excellent anti-settling property and excellent dispersibility. And the pretreatment is carried out in the water glass link through the accurate adding proportion, so that the quality stability of the terminal product is higher.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other examples, which a person of ordinary skill in the art would obtain without making any inventive effort based on the examples herein, are within the scope of the present invention, which is described by way of the following detailed description, but are not limited to the specific examples given below.
The invention provides a water glass pretreatment process, which comprises the following steps:
(1) Adding water glass with the modulus of 3.2-3.7 and water into a rotary spherical digester, and sealing;
(2) Introducing water vapor into the rotary spherical digester in the step (1) to ensure that the pressure in the rotary spherical digester reaches 0.08-0.15 MPa, and maintaining the pressure for 4-6 hours to obtain a water glass solution;
(3) And (3) feeding the water glass solution obtained in the step (2) into a middle-rotating dispersion tank, reducing the temperature to 75-90 ℃, adding a treating agent, and stirring for 20-60 minutes at the rotating speed of 70-110 r/min.
In a preferred embodiment, said step (3) is carried out by reducing the temperature to 78-85 ℃.
In a more preferred embodiment, the step (3) reduces the temperature to 80 ℃.
In a preferred embodiment, the stirring in step (3) is carried out for 30 minutes at a rotational speed of 100 revolutions per minute.
In a preferred embodiment, the mass ratio of the water glass to the water in the step (1) is (1.0-3.0): 1.5-6.0.
In a more preferred embodiment, the mass ratio of the water glass to the water in the step (1) is (1.0-2.0): 3.0-5.0.
In a more preferred embodiment, the mass ratio of water glass to water in the step (1) is 1:3.5.
water glass
Water glass is a silicate that is soluble in water. It is composed of alkali metal and silicon dioxide in different proportions. Most commonly used is sodium silicate water glass Na 2 O·nSiO 2 Also potassium silicate K 2 O·nSiO 2 . The molar ratio of silica to sodium oxide (or potassium oxide) in the water glass composition is generally referred to as the modulus M.
The water glass was purchased from Hangzhou Key bright building materials technology Co., ltd. Liquid water glass with a modulus of 3.2.
In a preferred embodiment, the pressure in the rotary spherical digester in the step (2) is 0.08-0.1 MPa.
In a more preferred embodiment, the pressure in the rotary spherical digester of step (2) is 0.1MPa.
The inventor finds that in the implementation process: the mass ratio of the water glass to the water is (1.0-3.0) (1.5-6.0), the pressure in the rotary spherical digester reaches 0.08-0.15 MPa, and the pressure is maintained for 4-6 hours; by dissolving the water glass, the dispersibility of the silica prepared at a later stage can be improved.
After the water glass is mixed with water, a series of hydrolysis reactions and ionization balances are produced, so that the solution contains sodium orthosilicate, sodium polysilicate, silicic acid, polysilicic acid and OH - 、Na + 、HSiO 3 - And complex colloid-molecule-ion system composed of various components. In the implementation process of the applicant, the water glass and water ratio is limited, and the pressure in the rotary spherical digester is set to be 0.08-0.15 MPa, so that the water glass can be dissolved, the dispersibility of the silicon dioxide prepared in the later stage can be improved, the water glass solution can form a colloid-molecule-ion system with a specific ratio by limiting the water glass and water ratio, and then the hydrolysis or ionization balance is promoted under the pressure of 0.08-0.15 MPa, so that the condensation polymerization of silicic acid into polysilicic acid colloidal particles or sodium orthosilicate is prevented to a certain extent, the colloidal particles are thinned, and the molecular weight of polysilicic acid is re-homogenized.
When the pressure is not between 0.08MPa and 0.15MPa or the mass ratio of water glass to water is not (1.0 to 3.0): 1.5 to 6.0, the prepared silicon dioxide has poor dispersibility because a colloid-molecule-ion system with a certain proportion is not obtained.
In a preferred embodiment, the mass of the treating agent in the step (3) is 1 to 4% of that of the water glass.
Treating agent
The treating agent is a substance for improving the adhesion property and is used for treating the surfaces of plastics, fillers, pigments, adhesion carriers and the like, and generally comprises paraffin, a coupling agent, a surfactant and the like.
Paraffin is mainly composed of alkane, is an inactive organic compound, and generally comprises oxidized paraffin, microcrystalline wax, oxidized microcrystalline wax, polyethylene wax, oxidized polyethylene wax and the like.
In a preferred embodiment, the treating agent of step (3) is selected from one or more of oxidized paraffin wax, oxidized microcrystalline wax, oxidized polyethylene wax.
The oxidized paraffin introduces oxygen-containing groups into the paraffin, so that a plurality of new characteristics of the paraffin are given, the application field of the paraffin is widened, and particularly the emulsifying property of the paraffin is greatly improved.
Oxidized microcrystalline waxes are the introduction of oxygen-containing groups into microcrystalline waxes that impart many new properties to microcrystalline waxes.
Microcrystalline wax, white amorphous solid wax, C 31-70 Branched saturated hydrocarbon of (2) is the main component, contains a small amount of cyclic and straight hydrocarbon, and is odorless and tasteless; is insoluble in ethanol, slightly soluble in hot ethanol, and soluble in benzene, chloroform, diethyl ether, etc.; is miscible with various mineral waxes, vegetable waxes and hot fatty oils. Mainly takes residue after petroleum fractionation as raw material, and is prepared by adopting a refining method.
Oxidized polyethylene wax, also known as OPE wax, is a low molecular weight ethylene-vinyl acetate copolymer containing carbonyl groups and hydroxyl groups; OPE wax has the special properties of low viscosity, high softening point, good hardness and the like, is nontoxic, good in thermal stability, low in high-temperature volatility, and excellent in dispersibility of filler and pigment, has excellent external lubricity, has strong internal lubricating effect and has coupling effect.
Examples of oxidized polyethylene waxes include, but are not limited to: high density oxidized polyethylene wax OPE316, oxidized polyethylene wax 629 (Honiswell wax powder), oxidized polyethylene wax OPE3715 (Craien), oxidized polyethylene wax AC316a (Honiswell wax powder).
In a preferred embodiment, the step (3) treatment agent is an oxidized polyethylene wax.
In a more preferred embodiment, the oxidized polyethylene wax is available from clahn under model number 3715.
The inventor finds that the addition of oxidized polyethylene wax can reduce the glossiness of the paint, and after the molecular weight of polysilicic acid is homogenized, the polar groups on the oxidized polyethylene wax are combined with the polysilicic acid, so that the surface energy of the polysilicic acid is reduced, and the further polymerization of the polysilicic acid is further limited; meanwhile, in the process of silicon dioxide generated by the reaction of the water glass solution modified by the oxidized polyethylene wax and the acid, polar groups on the oxidized polyethylene wax are adsorbed on the surface of the silicon dioxide to replace water combined with-OH on the surface of the silicon dioxide through hydrogen bonds, so that the formation of hydrogen bonds among silicon dioxide particles is prevented; meanwhile, nonpolar groups on the oxidized polyethylene wax are easy to permeate into the pores in the silicon dioxide, so that cohesion is weakened, the silicon dioxide is easier to open under the action of external force, and newly generated particles can be rapidly protected. The silicon dioxide is used for coating, and in the process of coating into a film and drying, the solvent and the resin base material are blocked by the chemical and physical actions of the silicon dioxide outer layer structure, so that the flow of the resin base material and the volatilization of the solvent are slowed down, and the glossiness of the coating is reduced. The silica-containing coating film is poor in blocking resistance due to the presence of the oxidized polyethylene wax.
In a preferred embodiment, the step (3) treatment agent further comprises an adjuvant.
In a preferred embodiment, the step (3) treatment agent is a combination of oxidized polyethylene wax and an adjuvant.
In a preferred embodiment, the adjuvant comprises 0.05 to 0.2wt% of the treating agent.
In a preferred embodiment, the auxiliary agent is one of a nonionic surfactant alkylphenol ethoxylate or a nonionic surfactant fatty alcohol ethoxylate.
In a preferred embodiment, the adjuvant is alkylphenol ethoxylates.
In a more preferred embodiment, the alkylphenol ethoxylates are selected from one or more of nonylphenol ethoxylate, pentylphenol ethoxylate, octylphenol ethoxylate, decylphenol ethoxylate, undecylphenol ethoxylate, dodecylphenol ethoxylate, pentadecylphenol ethoxylate.
In a more preferred embodiment, the alkylphenol ethoxylates are nonylphenol ethoxylate (CAS 127087-87-0), octylphenol ethoxylate (CAS 9002-93-1), pentadecylphenol ethoxylate (CAS 40160-92-7).
More preferably, the alkylphenol ethoxylates comprise 70-88% of the polyoxyethylene nonylphenol ether, more than 15% of the polyoxyethylene octylphenol ether and 2% of the polyoxyethylene pentadecylphenol ether by weight percent.
The silica produced by the reaction with the acid after the addition of the auxiliary agent can improve the anti-back tack of the coating film by crosslinking with the coating system. Moreover, the applicant has unexpectedly found that when the weight of the auxiliary agent is 0.05 to 0.2% of that of the oxidized polyethylene wax, the anti-settling property of the coating is improved, presumably for the following reasons: the nonylphenol polyoxyethylene ether, the octylphenol polyoxyethylene ether, the pentadecylphenol polyoxyethylene ether and the dinonylphenol polyoxyethylene ether are mutually cooperated with oxidized polyethylene wax to form a rigid three-dimensional network structure around the silicon dioxide, and when the silicon dioxide is dispersed in the coating, a stable structure is formed due to the fact that the density of the network structure is high and under the action of Van der Waals force; meanwhile, pseudo wetting particles formed in the stirring process are soaked for a short time, the silicon dioxide is fully wetted, the static viscosity of the product is increased, the sedimentation of the silicon dioxide is slowed down, and the layering phenomenon is avoided.
When the mass parts of the auxiliary agent are small, a stable network structure cannot be formed; in more cases, the formed network structure is dense, and silica cannot be fully wetted, so that the stability of the coating can be affected.
Example 1
The embodiment 1 of the invention provides a water glass pretreatment process, which comprises the following steps:
(1) Adding water glass and water into a rotary spherical digester, and sealing;
(2) Introducing steam into the rotary spherical digester in the step (1) to enable the pressure in the rotary spherical digester to reach 0.08MPa, and maintaining the pressure for 6 hours to obtain a water glass solution;
(3) And (3) feeding the water glass solution obtained in the step (2) into a middle-rotating dispersion tank, reducing the temperature by 80 ℃, adding a treating agent, and stirring for 30 minutes at the rotating speed of 100 rpm.
And (3) the mass ratio of the water glass to the water in the step (1) is 1:6.
The water glass is purchased from Hangzhou Key British building materials science and technology Co, and the modulus is 3.2.
The mass of the treating agent in the step (3) is 1% of that of the water glass.
The treating agent in the step (3) is a composition of oxidized polyethylene wax and an auxiliary agent.
The oxidized polyethylene wax was purchased from clariant under model number 3715.
The auxiliary agent comprises, by mass, 70% of nonylphenol polyoxyethylene ether, 28% or more of octylphenol polyoxyethylene ether and 2% of pentadecyl phenol polyoxyethylene ether.
The auxiliary agent accounts for 0.05wt% of the treating agent.
Example 2
The embodiment 2 of the invention provides a water glass pretreatment process, which comprises the following steps:
(1) Adding water glass and water into a rotary spherical digester, and sealing;
(2) Introducing steam into the rotary spherical digester in the step (1) to enable the pressure in the rotary spherical digester to reach 0.15MPa, and maintaining the pressure for 4 hours to obtain a water glass solution;
(3) And (3) feeding the water glass solution obtained in the step (2) into a middle-rotating dispersion tank, reducing the temperature by 80 ℃, adding a treating agent, and stirring for 30 minutes at the rotating speed of 100 rpm.
And (3) the mass ratio of the water glass to the water in the step (1) is 1:2.
The water glass is purchased from Hangzhou Key British building materials science and technology Co, and the modulus is 3.2.
The mass of the treating agent in the step (3) is 4% of that of the water glass.
The treating agent in the step (3) is a composition of oxidized polyethylene wax and an auxiliary agent.
The oxidized polyethylene wax was purchased from clariant under model number 3715.
The auxiliary agent comprises, by mass, 80% of nonylphenol polyoxyethylene ether, 18% or more of octylphenol polyoxyethylene ether and 2% of pentadecyl phenol polyoxyethylene ether.
The auxiliary agent accounts for 0.2wt% of the treating agent.
Example 3
The embodiment 3 of the invention provides a water glass pretreatment process, which comprises the following steps:
(1) Adding water glass and water into a rotary spherical digester, and sealing;
(2) Introducing steam into the rotary spherical digester in the step (1) to enable the pressure in the rotary spherical digester to reach 0.1MPa, and maintaining the pressure for 5 hours to obtain a water glass solution;
(3) And (3) feeding the water glass solution obtained in the step (2) into a middle-rotating dispersion tank, reducing the temperature by 80 ℃, adding a treating agent, and stirring for 30 minutes at the rotating speed of 100 rpm.
And (3) the mass ratio of the water glass to the water in the step (1) is 2:1.
The water glass is purchased from Hangzhou Key British building materials science and technology Co, and the modulus is 3.2.
The mass of the treating agent in the step (3) is 3% of that of the water glass.
The treating agent in the step (3) is a composition of oxidized polyethylene wax and an auxiliary agent.
The oxidized polyethylene wax was purchased from clariant under model number 3715.
The auxiliary agent comprises, by mass, 74% of polyoxyethylene nonylphenol ether, 24% or more of polyoxyethylene octylphenol ether and 2% of polyoxyethylene pentadecyl phenol ether.
The auxiliary agent accounts for 0.15wt% of the treating agent.
Example 4
The embodiment 4 of the invention provides a water glass pretreatment process, which comprises the following steps:
(1) Adding water glass and water into a rotary spherical digester, and sealing;
(2) Introducing steam into the rotary spherical digester in the step (1) to enable the pressure in the rotary spherical digester to reach 0.1MPa, and maintaining the pressure for 5 hours to obtain a water glass solution;
(3) And (3) feeding the water glass solution obtained in the step (2) into a middle-rotating dispersion tank, reducing the temperature by 80 ℃, adding a treating agent, and stirring for 30 minutes at the rotating speed of 100 rpm.
The mass ratio of the water glass to the water in the step (1) is 1:1.5.
The water glass is purchased from Hangzhou Key British building materials science and technology Co, and the modulus is 3.2.
The mass of the treating agent in the step (3) is 3% of that of the water glass.
The treating agent in the step (3) is a composition of oxidized polyethylene wax and an auxiliary agent.
The oxidized polyethylene wax was purchased from clariant under model number 3715.
The auxiliary agent comprises, by mass, 74% of polyoxyethylene nonylphenol ether, 24% or more of polyoxyethylene octylphenol ether and 2% of polyoxyethylene pentadecyl phenol ether.
The auxiliary agent accounts for 0.15wt% of the treating agent.
Example 5
The embodiment 5 of the invention provides a water glass pretreatment process, which comprises the following steps of:
(1) Adding water glass and water into a rotary spherical digester, and sealing;
(2) Introducing steam into the rotary spherical digester in the step (1) to enable the pressure in the rotary spherical digester to reach 0.1MPa, and maintaining the pressure for 5 hours to obtain a water glass solution;
(3) And (3) feeding the water glass solution obtained in the step (2) into a middle-rotating dispersion tank, reducing the temperature by 80 ℃, adding a treating agent, and stirring for 30 minutes at the rotating speed of 100 rpm.
The mass ratio of the water glass to the water in the step (1) is 1:3.5.
The water glass is purchased from Hangzhou Key British building materials science and technology Co, and the modulus is 3.2.
The mass of the treating agent in the step (3) is 3% of that of the water glass.
The treating agent in the step (3) is a composition of oxidized polyethylene wax and an auxiliary agent.
The oxidized polyethylene wax was purchased from clariant under model number 3715.
The auxiliary agent comprises, by mass, 74% of polyoxyethylene nonylphenol ether, 24% or more of polyoxyethylene octylphenol ether and 2% of polyoxyethylene pentadecyl phenol ether.
The auxiliary agent accounts for 0.15wt% of the treating agent.
Example 6
The embodiment 6 of the invention provides a water glass pretreatment process, which comprises the following steps:
(1) Adding water glass and water into a rotary spherical digester, and sealing;
(2) Introducing steam into the rotary spherical digester in the step (1) to enable the pressure in the rotary spherical digester to reach 2MPa, and maintaining the pressure for 5 hours to obtain a water glass solution;
(3) And (3) feeding the water glass solution obtained in the step (2) into a middle-rotating dispersion tank, reducing the temperature by 80 ℃, adding a treating agent, and stirring for 30 minutes at the rotating speed of 100 rpm.
The mass ratio of the water glass to the water in the step (1) is 1:3.5.
The water glass is purchased from Hangzhou Key British building materials science and technology Co, and the modulus is 3.2.
The mass of the treating agent in the step (3) is 3% of that of the water glass.
The treating agent in the step (3) is a composition of oxidized polyethylene wax and an auxiliary agent.
The oxidized polyethylene wax was purchased from clariant under model number 3715.
The auxiliary agent comprises, by mass, 74% of polyoxyethylene nonylphenol ether, 24% or more of polyoxyethylene octylphenol ether and 2% of polyoxyethylene pentadecyl phenol ether.
The auxiliary agent accounts for 0.15wt% of the treating agent.
Example 7
Embodiment 7 of the present invention provides a water glass pretreatment process, comprising the following steps:
(1) Adding water glass and water into a rotary spherical digester, and sealing;
(2) Introducing steam into the rotary spherical digester in the step (1) to enable the pressure in the rotary spherical digester to reach 0.05MPa, and maintaining the pressure for 5 hours to obtain a water glass solution;
(3) And (3) feeding the water glass solution obtained in the step (2) into a middle-rotating dispersion tank, reducing the temperature by 80 ℃, adding a treating agent, and stirring for 30 minutes at the rotating speed of 100 rpm.
The mass ratio of the water glass to the water in the step (1) is 1:3.5.
The water glass is purchased from Hangzhou Key British building materials science and technology Co, and the modulus is 3.2.
The mass of the treating agent in the step (3) is 3% of that of the water glass.
The treating agent in the step (3) is a composition of oxidized polyethylene wax and an auxiliary agent.
The oxidized polyethylene wax was purchased from clariant under model number 3715.
The auxiliary agent comprises, by mass, 74% of polyoxyethylene nonylphenol ether, 24% or more of polyoxyethylene octylphenol ether and 2% of polyoxyethylene pentadecyl phenol ether.
The auxiliary agent accounts for 0.15wt% of the treating agent.
Example 8
The embodiment 8 of the invention provides a water glass pretreatment process, which comprises the following steps of:
(1) Adding water glass and water into a rotary spherical digester, and sealing;
(2) Introducing steam into the rotary spherical digester in the step (1) to enable the pressure in the rotary spherical digester to reach 0.1MPa, and maintaining the pressure for 5 hours to obtain a water glass solution;
(3) And (3) feeding the water glass solution obtained in the step (2) into a middle-rotating dispersion tank, reducing the temperature by 80 ℃, adding a treating agent, and stirring for 30 minutes at the rotating speed of 100 rpm.
And (3) the mass ratio of the water glass to the water in the step (1) is 1:8.
The water glass is purchased from Hangzhou Key British building materials science and technology Co, and the modulus is 3.2.
The mass of the treating agent in the step (3) is 3% of that of the water glass.
The treating agent in the step (3) is a composition of oxidized polyethylene wax and an auxiliary agent.
The oxidized polyethylene wax was purchased from clariant under model number 3715.
The auxiliary agent comprises, by mass, 74% of polyoxyethylene nonylphenol ether, 24% or more of polyoxyethylene octylphenol ether and 2% of polyoxyethylene pentadecyl phenol ether.
The auxiliary agent accounts for 0.15wt% of the treating agent.
Example 9
Embodiment 9 of the present invention provides a water glass pretreatment process, comprising the following steps:
(1) Adding water glass and water into a rotary spherical digester, and sealing;
(2) Introducing steam into the rotary spherical digester in the step (1) to enable the pressure in the rotary spherical digester to reach 0.1MPa, and maintaining the pressure for 5 hours to obtain a water glass solution;
(3) And (3) feeding the water glass solution obtained in the step (2) into a middle-rotating dispersion tank, reducing the temperature by 80 ℃, adding a treating agent, and stirring for 30 minutes at the rotating speed of 100 rpm.
The mass ratio of the water glass to the water in the step (1) is 4:1.
The water glass is purchased from Hangzhou Key British building materials science and technology Co, and the modulus is 3.2.
The mass of the treating agent in the step (3) is 3% of that of the water glass.
The treating agent in the step (3) is a composition of oxidized polyethylene wax and an auxiliary agent.
The oxidized polyethylene wax was purchased from clariant under model number 3715.
The auxiliary agent comprises, by mass, 74% of polyoxyethylene nonylphenol ether, 24% or more of polyoxyethylene octylphenol ether and 2% of polyoxyethylene pentadecyl phenol ether.
The auxiliary agent accounts for 0.15wt% of the treating agent.
Example 10
The embodiment 10 of the invention provides a water glass pretreatment process, which comprises the following steps:
(1) Adding water glass and water into a rotary spherical digester, and sealing;
(2) Introducing steam into the rotary spherical digester in the step (1) to enable the pressure in the rotary spherical digester to reach 0.1MPa, and maintaining the pressure for 5 hours to obtain a water glass solution;
(3) And (3) feeding the water glass solution obtained in the step (2) into a middle-rotating dispersion tank, reducing the temperature by 80 ℃, adding a treating agent, and stirring for 30 minutes at the rotating speed of 100 rpm.
The mass ratio of the water glass to the water in the step (1) is 1:3.5.
The water glass is purchased from Hangzhou Key British building materials science and technology Co, and the modulus is 3.2.
The mass of the treating agent in the step (3) is 6% of that of the water glass.
The treating agent in the step (3) is a composition of oxidized polyethylene wax and an auxiliary agent.
The oxidized polyethylene wax was purchased from clariant under model number 3715.
The auxiliary agent comprises, by mass, 74% of polyoxyethylene nonylphenol ether, 24% or more of polyoxyethylene octylphenol ether and 2% of polyoxyethylene pentadecyl phenol ether.
The auxiliary agent accounts for 0.15wt% of the treating agent.
Example 11
Embodiment 11 of the present invention provides a water glass pretreatment process, comprising the following steps:
(1) Adding water glass and water into a rotary spherical digester, and sealing;
(2) Introducing steam into the rotary spherical digester in the step (1) to enable the pressure in the rotary spherical digester to reach 0.1MPa, and maintaining the pressure for 5 hours to obtain a water glass solution;
(3) And (3) feeding the water glass solution obtained in the step (2) into a middle-rotating dispersion tank, reducing the temperature by 80 ℃, adding a treating agent, and stirring for 30 minutes at the rotating speed of 100 rpm.
The mass ratio of the water glass to the water in the step (1) is 1:3.5.
The water glass is purchased from Hangzhou Key British building materials science and technology Co, and the modulus is 3.2.
The mass of the treating agent in the step (3) is 0.1% of that of the water glass.
The treating agent in the step (3) is a composition of oxidized polyethylene wax and an auxiliary agent.
The oxidized polyethylene wax was purchased from clariant under model number 3715.
The auxiliary agent comprises, by mass, 74% of polyoxyethylene nonylphenol ether, 24% or more of polyoxyethylene octylphenol ether and 2% of polyoxyethylene pentadecyl phenol ether.
The auxiliary agent accounts for 0.15wt% of the treating agent.
Example 12
Embodiment 12 of the present invention provides a water glass pretreatment process, comprising the following steps:
(1) Adding water glass and water into a rotary spherical digester, and sealing;
(2) Introducing steam into the rotary spherical digester in the step (1) to enable the pressure in the rotary spherical digester to reach 0.1MPa, and maintaining the pressure for 5 hours to obtain a water glass solution;
(3) And (3) feeding the water glass solution obtained in the step (2) into a middle-rotating dispersion tank, reducing the temperature by 80 ℃, adding a treating agent, and stirring for 30 minutes at the rotating speed of 100 rpm.
The mass ratio of the water glass to the water in the step (1) is 1:3.5.
The water glass is purchased from Hangzhou Key British building materials science and technology Co, and the modulus is 3.2.
The mass of the treating agent in the step (3) is 3% of that of the water glass.
The treating agent in the step (3) is a composition of oxidized polyethylene wax and an auxiliary agent.
The oxidized polyethylene wax was purchased from clariant under model number 3715.
The auxiliary agent comprises, by mass, 74% of polyoxyethylene nonylphenol ether, 24% or more of polyoxyethylene octylphenol ether and 2% of polyoxyethylene pentadecyl phenol ether.
The auxiliary agent accounts for 3wt% of the treating agent.
Example 13
Embodiment 13 of the present invention provides a water glass pretreatment process, comprising the following steps:
(1) Adding water glass and water into a rotary spherical digester, and sealing;
(2) Introducing steam into the rotary spherical digester in the step (1) to enable the pressure in the rotary spherical digester to reach 0.1MPa, and maintaining the pressure for 5 hours to obtain a water glass solution;
(3) And (3) feeding the water glass solution obtained in the step (2) into a middle-rotating dispersion tank, reducing the temperature by 80 ℃, adding a treating agent, and stirring for 30 minutes at the rotating speed of 100 rpm.
The mass ratio of the water glass to the water in the step (1) is 1:3.5.
The water glass is purchased from Hangzhou Key British building materials science and technology Co, and the modulus is 3.2.
The mass of the treating agent in the step (3) is 3% of that of the water glass.
The treating agent in the step (3) is a composition of oxidized polyethylene wax and an auxiliary agent.
The oxidized polyethylene wax was purchased from clariant under model number 3715.
The auxiliary agent is nonylphenol polyoxyethylene ether.
The auxiliary agent accounts for 0.15wt% of the treating agent.
Example 14
Embodiment 14 of the present invention provides a water glass pretreatment process, comprising the following steps:
(1) Adding water glass and water into a rotary spherical digester, and sealing;
(2) Introducing steam into the rotary spherical digester in the step (1) to enable the pressure in the rotary spherical digester to reach 0.1MPa, and maintaining the pressure for 5 hours to obtain a water glass solution;
(3) And (3) feeding the water glass solution obtained in the step (2) into a middle-rotating dispersion tank, reducing the temperature by 80 ℃, adding a treating agent, and stirring for 30 minutes at the rotating speed of 100 rpm.
The mass ratio of the water glass to the water in the step (1) is 1:3.5.
The water glass is purchased from Hangzhou Key British building materials science and technology Co, and the modulus is 3.2.
The mass of the treating agent in the step (3) is 3% of that of the water glass.
The treating agent in the step (3) is a composition of oxidized polyethylene wax and an auxiliary agent.
The oxidized polyethylene wax was purchased from clariant under model number 3715.
The auxiliary agent is pentadecyl phenol polyoxyethylene ether.
The auxiliary agent accounts for 0.15wt% of the treating agent.
Example 15
Embodiment 15 of the present invention provides a water glass pretreatment process, comprising the following steps:
(1) Adding water glass and water into a rotary spherical digester, and sealing;
(2) Introducing steam into the rotary spherical digester in the step (1) to enable the pressure in the rotary spherical digester to reach 0.1MPa, and maintaining the pressure for 5 hours to obtain a water glass solution;
(3) And (3) feeding the water glass solution obtained in the step (2) into a middle-rotating dispersion tank, reducing the temperature by 80 ℃, adding a treating agent, and stirring for 30 minutes at the rotating speed of 100 rpm.
The mass ratio of the water glass to the water in the step (1) is 1:3.5.
The water glass is purchased from Hangzhou Key British building materials science and technology Co, and the modulus is 3.2.
The mass of the treating agent in the step (3) is 3% of that of the water glass.
The treating agent in the step (3) is a composition of oxidized polyethylene wax and an auxiliary agent.
The oxidized polyethylene wax was purchased from clariant under model number 3715.
The auxiliary agent is octyl phenol polyoxyethylene ether.
The auxiliary agent accounts for 0.15wt% of the treating agent.
Example 16
Embodiment 16 of the present invention provides a water glass pretreatment process, comprising the following steps:
(1) Adding water glass and water into a rotary spherical digester, and sealing;
(2) Introducing steam into the rotary spherical digester in the step (1) to enable the pressure in the rotary spherical digester to reach 0.1MPa, and maintaining the pressure for 5 hours to obtain a water glass solution;
(3) And (3) feeding the water glass solution obtained in the step (2) into a middle-rotating dispersion tank, reducing the temperature by 80 ℃, adding a treating agent, and stirring for 30 minutes at the rotating speed of 100 rpm.
The mass ratio of the water glass to the water in the step (1) is 1:3.5.
The water glass is purchased from Hangzhou Key British building materials science and technology Co, and the modulus is 3.2.
The mass of the treating agent in the step (3) is 3% of that of the water glass.
The treating agent in the step (3) is a composition of oxidized polyethylene wax and an auxiliary agent.
The oxidized polyethylene wax was purchased from clariant under model number 3715.
The auxiliary agent comprises, by mass, 74% of polyoxyethylene nonylphenol ether, 24% or more of polyoxyethylene octylphenol ether and 2% of polyoxyethylene undecylenate.
The auxiliary agent accounts for 0.15wt% of the treating agent.
Performance evaluation:
the water glass obtained in examples 1 to 16 was reacted with sulfuric acid to prepare silica, the preparation method was a conventional preparation method, and the preparation conditions of silica in the following test were: 8 volumes of water glass solution are reacted with 1 volume of sulfuric acid, aged for 2 hours at a constant temperature of 80 ℃, and dried for 1 hour at 400 ℃.
Testing the anti-tack, gloss, and anti-settling performance test required that the silica be placed into the following coating for testing.
The formula of the coating comprises the following steps:
main paint:
| component name | Mass content% |
| Acrylic resin | 74.4％ |
| Leveling agent BYK323 | 0.46％ |
| Leveling agent BYK333 | 0.46％ |
| Defoaming agent BYK141 | 0.27％ |
| Polybasic acetate BAC | 17.39％ |
| Silica dioxide | 7％ |
Curing agent:
| curing agent AK-75 | 41％ |
| Curing agent TR-50 | 18％ |
| Polybasic acetate BAC | 41％ |
Dispersibility of
The testing method comprises the following steps: and (3) testing by using a sanding and dispersing machine, wherein silicon dioxide is pumped into paint, the rotating speed of the sanding and dispersing machine is 1600r/min, and the dispersing time is recorded.
Anti-tack
Test conditions: the quantitative filter paper sheet is placed on a paint film which is not less than 1cm away from the edge of a sample plate in a smooth face down manner according to the relevant regulations of GB/T1762-1980 paint film back tack measurement method, the quantitative filter paper sheet is placed in a constant temperature and humidity box, a back tack tester which is preheated under the conditions that the temperature is regulated to 40+/-1 ℃ and the relative humidity is 80+/-2% is placed in the center of the filter paper, and the constant temperature and humidity box is closed. The temperature was raised to 40.+ -. 1 ℃ and the relative humidity 80.+ -. 2% within 5 minutes, and the reaction was maintained under this condition for 10 minutes. And quickly taking the tester upwards and taking out the sample plate. The mixture was left for 15 minutes, and the result was observed with a four-fold magnifying glass.
Evaluation criteria: the template is inverted, the filter paper sheet does free falling motion, or the filter paper sheet can fall down by tapping with the index finger of a holding wrench; gently lifting the filter paper sheet, allowing an imprint, sticking sparse, slightly filter paper fibers with total fiber area of 1/3cm 2 The following is grade 2, the filter paper sheet is lifted gently, the ink is allowed to be stamped, dense filter paper fibers are stuck, and the total area is 1/3cm 2 ～1/2cm 2 And is level 3.
In the test, three templates are prepared for each sample at the same time for measurement, and the grade of 2 consistent results is taken as the evaluation result.
Gloss level
Test conditions: the test angle was 60℃as specified in GB/T9754-2007 relating to the determination of 20℃60℃and 85℃specular gloss of paint films of metallic pigment-free paint films.
Sinking resistance
The experiment environment is set to be 25.8 ℃ and 70% of humidity, and the water glass is placed in the paint and placed at room temperature for 10 hours to analyze the anti-sinking property of the paint
According to the performance verification method provided by the invention, the dispersibility, the anti-tack property, the glossiness and the anti-sinking property of the water glass after the pretreatment process in examples 1 to 8 are measured, and the results are shown in Table 1.
TABLE 1
The description and the application of the present invention are illustrative, and it is not intended to limit the scope of the invention to the above-described embodiments, and therefore, the invention is not limited to the embodiments, and any technical solution obtained by adopting equivalent substitution is within the scope of the protection of the invention.
Claims (4)
1. A water glass pretreatment process is characterized in that: the pretreatment process comprises the following steps:
(1) Adding water glass with the modulus of 3.2-3.7 and water into a rotary spherical digester, and sealing;
(2) Introducing water vapor into the rotary spherical digester in the step (1) to ensure that the pressure in the rotary spherical digester reaches 0.08-0.15 MPa, and maintaining the pressure for 4-6 hours to obtain a water glass solution;
(3) Feeding the water glass solution obtained in the step (2) into a middle-rotating dispersion tank, reducing the temperature to 75-90 ℃, adding a treating agent, and stirring for 20-60 minutes at the rotating speed of 70-110 r/min;
the mass ratio of the water glass to the water in the step (1) is (1.0-3.0): 1.5-6.0;
the treating agent in the step (3) comprises oxidized polyethylene wax, and the mass of the treating agent is 1-4% of that of water glass;
the treating agent in the step (3) also comprises an auxiliary agent, wherein the auxiliary agent accounts for 0.05-0.2 wt% of the treating agent;
the auxiliary agent is alkylphenol ethoxylate, wherein the alkylphenol ethoxylate is a mixture of three types of polyoxyethylene ether which are combined together, namely 70-88% of polyoxyethylene ether of union-based phenol, more than 15% of polyoxyethylene ether of octyl-phenol and 2% of polyoxyethylene ether of pentadecyl-phenol;
the water glass is subjected to a pretreatment process and then reacts with sulfuric acid to prepare silicon dioxide for the paint.
2. A water glass pretreatment process according to claim 1, wherein: the mass ratio of the water glass to the water in the step (1) is (1.0-2.0) and (3.0-5.0).
3. A water glass pretreatment process according to claim 1, wherein: the pressure in the rotary spherical digester in the step (2) is 0.08-0.1 MPa.
4. A water glass pretreatment process according to claim 1, wherein: the temperature is reduced to 78-85 ℃ in the step (3).
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| US3961022A (en) * | 1973-11-14 | 1976-06-01 | Philadelphia Quartz Company | Silicate dissolving |
| CN1541186A (en) * | 2001-08-13 | 2004-10-27 | ���ǻ�ѧ��˾ | Method of preparing silicas, silicas with specific pore-size distribution and use thereof in particular for reinforcing polymers |
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