CN105542512B - A kind of preparation method of water base zinc titanium composite mortar - Google Patents

A kind of preparation method of water base zinc titanium composite mortar Download PDF

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CN105542512B
CN105542512B CN201610077932.5A CN201610077932A CN105542512B CN 105542512 B CN105542512 B CN 105542512B CN 201610077932 A CN201610077932 A CN 201610077932A CN 105542512 B CN105542512 B CN 105542512B
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zinc
titanium composite
preparation
titanium
water base
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CN105542512A (en
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姚超
李俊乾
左士祥
刘文杰
吴凤芹
罗士平
李霞章
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Jiangsu Kona New Materials Co.,Ltd.
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Changzhou University
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    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/0081—Composite particulate pigments or fillers, i.e. containing at least two solid phases, except those consisting of coated particles of one compound
    • C09C1/0084—Composite particulate pigments or fillers, i.e. containing at least two solid phases, except those consisting of coated particles of one compound containing titanium dioxide
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    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/36—Compounds of titanium
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    • C09C1/3623—Grinding
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    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/36—Compounds of titanium
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    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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    • C09C1/3669—Treatment with low-molecular organic compounds
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    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/36—Compounds of titanium
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    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/06—Treatment with inorganic compounds
    • C09C3/063—Coating
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    • C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
    • C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
    • C01P2004/84—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases one phase coated with the other

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Abstract

The invention provides a kind of preparation method of water base zinc titanium composite mortar, by carrying out Ludox coating processing to zinc titanium composite mortar, it can not only effectively suppress the photochemical activity of zinc oxide and titanium oxide and the generation flocculated, lump and precipitated caused by zinc ion dissolution in zinc titanium composite mortar can also be suppressed.The water base zinc titanium composite mortar prepared through coating processing has the dual property of nano titanium oxide and nano zine oxide concurrently, and good shielding properties is respectively provided with to UVA and UVB, has widened its application in fields such as industry, daily use chemicals.

Description

A kind of preparation method of water base zinc-titanium composite mortar
Technical field
The invention belongs to composite function nano field of material preparation, and in particular to a kind of system of water base zinc-titanium composite mortar Preparation Method.
Background technology
In the light come out due to solar radiation, about 5% 200~400nm of wavelength ultraviolet there are (referred to as UV).Ultraviolet in sunshine, it can be divided into by its wavelength：320~400nm long wave ultraviolet (abbreviation UVA), 280~ 320nm ultraviolet B radiation (abbreviation UVB) and wavelength is 200~280nm short wave ultraviolet (abbreviation UVC).Wherein UVC because Wavelength is short, and penetrability is not strong, its 98% by earth stratosphere when, absorbed by ozone layer, the harm to the mankind is little.And UVB and UVA penetrability is stronger, the problems such as triggering blackspot, erythema, chafing to the long-term irradiation of human body, when serious even Cutaneum carcinoma can be caused.
Nano zine oxide and titanium oxide are two kinds of widely used inorganic UV shield agents, but they are to UVA's and UVB Screening ability is different：Nano-titanium oxide barrier UVB effect is very good but not good enough to UVA shield effectiveness；It is nano oxidized Zinc is undesirable to UVB shield effectiveness, but it obstructs UVA effects and is better than nano titanium oxide.In order to effectively shield UVA and UVB, reach the purpose of all band ultraviolet protection, usually need to add simultaneously in sun care preparations and high-molecular organic material to receive Rice titanium dioxide and nano zine oxide.
But due to nano zine oxide and the characteristic of semiconductor of titanium dioxide, under sunshine irradiation, its valence-band electrons is inhaled Receive ultraviolet to be excited and transit on conduction band, while produce hole-electron pair.Partial holes-electronics is to moving to semiconductor Surface, its surface hydroxyl and the hydrone of absorption is set to produce hydroxyl oxygen radical, hydroxyl oxygen radical has extremely strong oxidation susceptibility, meeting Make the organic matter degradation around it.Along with nano particle diameter is smaller, hole-electron is set to shorten the time for migrating surface, Reduce electronics and probability that hole recombines, therefore nano-oxide has very strong photochemical activity.In order to suppress oxygen Change zinc, the photochemical activity of titanium oxide need to be surface-treated it, and additionally, due to the property of zinc oxide two, Harvey Brown exist Illustrated in its book " property of zinc oxide and application " (International Lead Zinc Research Organization) Zinc oxide shows the activity with the multiple material of the salt and alkaline matter of acid and acid in water, causes zinc ion (Zn2+) easily Dissolution, the presence of a large amount of zinc ions can increase the viscosity of application system, or even make application system flocculation, caking and precipitation, this Using effect will be caused to be deteriorated with ultraviolet screener performance to decline.So zinc ion can be reduced in its Surface coating inoranic membrane Dissolution, the photochemical activity site for suppressing semiconductor.
At present, typically with silica, aluminum oxide, to titanium oxide, either zinc oxide carries out one-component, bi-component or multicomponent Coating processing.It is very common to the processing of the coating of titanium oxide, effect is all obvious, but the coating processing to zinc oxide but seems Deficiency.Coating is carried out to zinc oxide surface using silica as Chinese patent CN101024737A propositions are a kind of, its process is with silicon Hydrochlorate and sulfuric acid are raw material, but due to the highly acid of sulfuric acid, cause local acid dense due to having little time diffusion during dropwise addition Zinc oxide solution modeling zinc ion when spending big, because whole system is in alkaline environment, precipitation reaction generation occurs for zinc ion Zinc hydroxide, Zinc oxide water compound, it can so have a strong impact on uniformity, the compactness of clad.Hong Ruoyu is in research nano oxygen (Chinese powder technology, the 4th phase in 2005) using aluminum sulfate and sodium hydroxide as raw material, takes zinc oxide point when changing zinc coated aluminum oxide Part of sulfuric acid aluminium is first added after 60~80 DEG C of dispersion liquid heating, then sodium hydroxide adjusts system pH=9~10, maintains 1~2 hour, Then system pH is adjusted to be reacted 0.5 hour to neutrality with aluminum sulfate.Although this method will not cause surface of nanometer zinc oxide zinc ion Precipitation, it is but not very good to the inhibition of the photocatalytic activity of nano zine oxide.Chinese patent CN1253513C A kind of method in the coating hydrous silica of surface of nanometer zinc oxide, hydrated alumina or hydrated ferric oxide is proposed, due to the party Hydrochloric acid, sulfuric acid, acetic acid and the ammoniacal liquor used during method cladding can all cause the dissolving of nano zine oxide, zinc ion dissolution, lead Cause covered effect not good enough.
Therefore, studying zinc oxide and the process for treating surface and its dispersion technology of the composite particles containing zinc oxide has important meaning Justice, while study precondition and application that the scattered of nano combined slurries, stability will be further raising material properties Basis.
The content of the invention
The technical problem to be solved in the present invention is in background technology is overcome the shortcomings of, there is provided one kind can effectively suppress zinc The dissolution of ion, and can suppress the method for coating in the photochemical activity site of semi-conductor nano particles well.
The technical scheme is that：The zinc titanium composite wood prepared with Chinese patent CN200810243732.8 methods describeds Expect for raw material, by slurrying, the technique such as Ludox coating is completed.
The preparation method of the present invention uses following characteristics step：
1st, the preparation of zinc-titanium composite dispersion liquid：1~15% wetting dispersing agent is added in deionized water (presses powder quality Meter) stir, zinc-titanium composite granule is added, is stirred, it is 8~10 to adjust dispersion liquid pH value with organic amine, is then ground Produce zinc-titanium composite dispersion liquid.
2nd, prepared by Ludox：Deionized water is warming up to 75~95 DEG C, adjusts its pH value as 8~10, stir while 0.1~1.5mol/L sodium silicate solution is added dropwise, while the acid solution that 0.1~2.0mol/L is added dropwise maintains the pH constant, drips During adding solution by colourless gradually into transparent light oyster white colloidal sol, it is standby.
3rd, coating is handled：Zinc titanium composite dispersion liquid in step (1) is added to the silicon that step (2) obtains under stirring In colloidal sol, be incubated 0.5~1h, then 75~95 DEG C of temperature, pH value be stir for 8~10 times while be added dropwise 0.1~ 1.5mol/L sodium silicate solution, while the acid solution that 0.1~2.0mol/L is added dropwise maintains the pH constant, after adding, protects 0.5~1h of temperature.Then suspension is filtered and is washed with deionized to the μ S/cm of filtrate electrical conductivity≤200, obtain coating processing The compound filter cake of zinc-titanium.
4th, the preparation of water base zinc-titanium composite mortar：The compound filter cake of zinc titanium that step (3) is obtained after coating processing is divided again Dissipate, the preservative of addition 0.5~1% stirs (based on dispersion liquid quality), then grinds and water base zinc-titanium composite pulp is made Material.
Wetting dispersing agent in described step (1) is：Polycarboxylate sodium's class, special polycarboxylic acids ammonium salt class, polyacrylic acid One or more in sodium salt, polycarboxylic ethers；
Organic amine in described step (1) is：One kind or several in triethanolamine, isopropanolamine, diisopropanolamine (DIPA) Kind；
The mass concentration of Ludox in described step (2) is 0.1~0.5g/mL；
Acid solution in described step (2) and step (3) is：One kind or its mixing in hydrochloric acid, sulfuric acid, nitric acid is molten Liquid；
The mass ratio of amount of sodium silicate and zinc-titanium composite granule is 0.05~0.3 in described step (3):1 (with silicic acid The oxide S iO of sodium2Meter)；
Milling apparatus in described step (1) and step (4) is：In sand mill, ball mill, ultrasonic cell disruptor One kind；
Preservative in described step (4) is：Benzoic acid and salt, sorbic acid and salt, Phenoxyethanol, diacetic acid One kind in sodium, calcium propionate, sodium lactate.
The beneficial effects of the present invention are：
The present invention is prepared for a kind of water base zinc-titanium composite mortar using zinc titanium composite material as raw material by coating process, its Advantage is：
1. being covered in zinc titanium composite mortar particle surface using the network structure of Ludox, then pass through the acid of sodium metasilicate again Solution is further compensated for because Ludox coats uneven unsound shortcoming, and this coating process effectively inhibits zinc oxide With the photochemical activity of titanium oxide and can also suppress in zinc titanium composite mortar to wad a quilt with cotton caused by zinc ion dissolution well The generation of solidifying, caking and precipitation；2. the water base zinc-titanium composite mortar prepared has pair of nano titanium oxide and nano zine oxide concurrently Principal characteristic energy, good shield effectiveness is respectively provided with to UVA and UVB；3. the preparation of water base zinc-titanium composite mortar has widened it in work The application in the fields such as industry, daily use chemicals.
Embodiment
With reference to specific embodiment, the present invention is furture elucidated, it should be understood that these embodiments are merely to illustrate the present invention Rather than limitation the scope of the present invention, after the present invention has been read, various equivalences of the those skilled in the art to the present invention The modification of form falls within the application appended claims limited range.
The good and bad of coating effect is evaluated by detecting before and after coating in filtrate zinc ion concentration in the present invention, wherein filtrate Middle zinc ion concentration is measured with the Vista-AX types plasma emission spectrum of Varian companies of the U.S..
Embodiment 1
1st, the preparation of zinc-titanium composite dispersion liquid：0.08kg wetting dispersing agent is added in 1.42kg deionized water PA25 stirs (based on powder quality), then adds 1kg zinc-titanium composite granule, stirs, it is adjusted with triethanolamine PH value is 9, obtains the compound pre-dispersed liquid of zinc-titanium, then grinds the compound pre-dispersed liquid of zinc-titanium by sand mill and zinc-titanium is made Composite dispersion liquid.
2nd, prepared by Ludox：Deionized water is warming up to 85 DEG C, its pH value is adjusted and is stirred for 10 while being added dropwise 0.8mol/L sodium silicate solution, while 1.0mol/L hydrochloric acid solution is added dropwise to maintain pH constant, during dropwise addition solution by Colourless is gradually that 0.3g/mL Ludox is standby into transparent light oyster white colloidal sol, obtained concentration.
3rd, coating is handled：Obtained Ludox 0.389L stirrings in step (2) are taken to be warming up to 85 DEG C, then by step (1) In obtained zinc-titanium composite dispersion liquid added under stirring in above-mentioned Ludox and be incubated 0.5h, then stir while 0.82L 0.8mol/L sodium silicate solutions are added dropwise, while add 1.0mol/L hydrochloric acid solutions to maintain pH constant, after adding, insulation 0.5h.Then suspension is filtered and is washed with deionized the zinc-titanium for the μ S/cm of filtrate electrical conductivity 134, obtaining coating and handling Compound filter cake.
4th, the preparation of water base zinc-titanium composite mortar：By the compound filter cake of zinc-titanium after the coating obtained in step (3) processing Again disperse in deionized water, the preservative Phenoxyethanol for adding 18.75g stirs (based on dispersion liquid quality), then Ground by sand mill and water base zinc-titanium composite mortar is made.
Embodiment 2
1st, the preparation of zinc-titanium composite dispersion liquid：0.01kg wetting dispersing agent is added in 1.49kg deionized water 5040 stir (based on powder quality), then add 1kg zinc-titanium composite granule, stir, it is adjusted with isopropanolamine PH value is 9, obtains the compound pre-dispersed liquid of zinc-titanium, then grinds the compound pre-dispersed liquid of zinc-titanium by ball mill and zinc-titanium is made Composite dispersion liquid.
2nd, prepared by Ludox：Deionized water is warming up to 75 DEG C, its pH value is adjusted and is stirred for 9 while being added dropwise 1.5mol/L sodium silicate solution, while 2.0mol/L sulfuric acid solution is added dropwise to maintain pH constant, during dropwise addition solution by Colourless is gradually that 0.5g/mL Ludox is standby into transparent light oyster white colloidal sol, obtained concentration.
3rd, coating is handled：Obtained Ludox 0.4L stirrings in step (2) are taken to be warming up to 75 DEG C, then by step (1) Obtained zinc-titanium composite dispersion liquid, which is added under stirring in above-mentioned Ludox, is incubated 0.75h, then stirs while dripping Add 1.11L 1.5mol/L sodium silicate solutions, while 2.0mol/L sulfuric acid solutions are added dropwise to maintain pH constant, after adding, insulation 0.75h.Then by suspension filter and be washed with deionized to the μ S/cm of filtrate electrical conductivity 167, obtain coating processing zinc- The compound filter cake of titanium.
4th, the preparation of water base zinc-titanium composite mortar：By the compound filter cake of zinc-titanium after the coating obtained in step (3) processing Again disperse in deionized water, the preservative sorbic acid for adding 25g stirs (based on dispersion liquid quality), then passes through ball Water base zinc-titanium composite mortar is made in grinding machine grinding.
Embodiment 3
1st, the preparation of zinc-titanium composite dispersion liquid：0.15kg wetting dispersing agent 752 is added in 1.35kg deionized water Stirred (based on powder quality), then add 1kg zinc-titanium composite granule, stir, its pH is adjusted with diisopropanolamine (DIPA) It is worth for 8, obtains the compound pre-dispersed liquid of zinc-titanium, then by ultrasonic cell disruptor by the compound pre-dispersed liquid grinding system of zinc-titanium Obtain zinc-titanium composite dispersion liquid.
2nd, prepared by Ludox：Deionized water is warming up to 95 DEG C, its pH value is adjusted and is stirred for 8 while being added dropwise 0.8mol/L sodium silicate solution, while 1.0mol/L salpeter solution is added dropwise to maintain pH constant, during dropwise addition solution by Colourless is gradually that 0.1g/mL Ludox is standby into transparent light oyster white colloidal sol, obtained concentration.
3rd, coating is handled：Obtained Ludox 0.333L stirrings in step (2) are taken to be warming up to 95 DEG C, then by step (1) In obtained zinc-titanium composite dispersion liquid added under stirring in above-mentioned Ludox and be incubated 1h, then stir while dripping Add 2.78L 0.1mol/L sodium silicate solutions, while 0.1mol/L salpeter solutions are added dropwise to maintain pH constant, after adding, insulation 1h.Then by suspension filter and be washed with deionized to the μ S/cm of filtrate electrical conductivity 183, obtain coating processing zinc-titanium it is multiple Close filter cake.
4th, the preparation of water base zinc-titanium composite mortar：By the compound filter cake of zinc-titanium after the coating obtained in step (3) processing Again disperse in deionized water, the preservative sodium lactate for adding 12.5g stirs (based on dispersion liquid quality), then passes through Water base zinc-titanium composite mortar is made in ultrasonic cell disruptor grinding.
Embodiment 4
1st, the preparation of zinc-titanium composite dispersion liquid：0.08kg wetting dispersing agent is added in 1.42kg deionized water 5060 stir (based on powder quality), then add 1kg zinc-titanium composite granule, stir, it is adjusted with triethanolamine PH value is 10, obtains the compound pre-dispersed liquid of zinc-titanium, then grinds the compound pre-dispersed liquid of zinc-titanium by sand mill and zinc-titanium is made Composite dispersion liquid.
2nd, prepared by Ludox：Deionized water is warming up to 75 DEG C, its pH value is adjusted and is stirred for 10 while being added dropwise 0.8mol/L sodium silicate solution, while 1.0mol/L hydrochloric acid solution is added dropwise to maintain pH constant, during dropwise addition solution by Colourless is gradually that 0.3g/mL Ludox is standby into transparent light oyster white colloidal sol, obtained concentration.
3rd, coating is handled：Obtained Ludox 0.389L stirrings in step (2) are taken to be warming up to 75 DEG C, then by step (1) In obtained zinc-titanium composite dispersion liquid added under stirring in above-mentioned Ludox and be incubated 0.5h, then stir while 0.82L 0.8mol/L sodium silicate solutions are added dropwise, while 1.0mol/L hydrochloric acid solutions are added dropwise to maintain pH constant, after adding, protect Warm 0.75h.Then suspension is filtered and is washed with deionized to the μ S/cm of filtrate electrical conductivity 189, obtain coating processing The compound filter cake of zinc-titanium.
4th, the preparation of water base zinc-titanium composite mortar：By the compound filter cake of zinc-titanium after the coating obtained in step (3) processing Again disperse in deionized water, the preservative benzoic acid for adding 18.75g stirs (based on dispersion liquid quality), Ran Houtong Cross sand mill grinding and water base zinc-titanium composite mortar is made.
Embodiment 5
1st, the preparation of zinc-titanium composite dispersion liquid：0.15kg wetting dispersing agent is added in 1.35kg deionized water PA25 stirs (based on powder quality), then adds 1kg zinc-titanium composite granule, stirs, adjusted with diisopropanolamine (DIPA) Its pH value is 8, obtains the compound pre-dispersed liquid of zinc-titanium, is then ground the compound pre-dispersed liquid of zinc-titanium by ultrasonic cell disruptor Grind to obtain zinc-titanium composite dispersion liquid.
2nd, prepared by Ludox：Deionized water is warming up to 95 DEG C, its pH value is adjusted and is stirred for 8 while being added dropwise 0.8mol/L sodium silicate solution, while 1.0mol/L sulfuric acid solution is added dropwise to maintain pH constant, during dropwise addition solution by Colourless is gradually that 0.1g/mL Ludox is standby into transparent light oyster white colloidal sol, obtained concentration.
3rd, coating is handled：Obtained Ludox 0.333L stirrings in step (2) are taken to be warming up to 95 DEG C, then by step (1) In obtained zinc-titanium composite dispersion liquid added under stirring in above-mentioned Ludox and be incubated 0.75h, then stir while 2.78L 0.1mol/L sodium silicate solutions are added dropwise, while 0.1mol/L sulfuric acid solutions are added dropwise to maintain pH constant, after adding, protect Warm 0.75h.Then suspension is filtered and is washed with deionized to the μ S/cm of filtrate electrical conductivity 117, obtain coating processing The compound filter cake of zinc-titanium.
4th, the preparation of water base zinc-titanium composite mortar：By the compound filter cake of zinc-titanium after the coating obtained in step (3) processing Again disperse in deionized water, the preservative sodium lactate for adding 12.5g stirs (based on dispersion liquid quality), then passes through Water base zinc-titanium composite mortar is made in ultrasonic cell disruptor grinding.
Comparative example 1
Ludox coating process is used after coating process in step (3) in embodiment 1 first is used into sodium metasilicate coating in comparative example, For other operating conditions with embodiment 1, concrete operations are as described below：
1st, the preparation of zinc-titanium composite dispersion liquid：0.08kg wetting dispersing agent is added in 1.42kg deionized water PA25 stirs (based on powder quality), then adds 1kg zinc-titanium composite granule, stirs, it is adjusted with triethanolamine PH value is 9, obtains the compound pre-dispersed liquid of zinc-titanium, then grinds the compound pre-dispersed liquid of zinc-titanium by sand mill and zinc-titanium is made Composite dispersion liquid.
2nd, prepared by Ludox：Deionized water is warming up to 85 DEG C, its pH value is adjusted and is stirred for 10 while being added dropwise 0.8mol/L sodium silicate solution, while 1.0mol/L hydrochloric acid solution is added dropwise to maintain pH constant, during dropwise addition solution by Colourless is gradually that 0.3g/mL Ludox is standby into transparent light oyster white colloidal sol, obtained concentration.
3rd, coating is handled：Zinc in step (1)-titanium composite dispersion liquid is warming up to 85 DEG C, then stirred while dripping Add 0.82L 0.8mol/L sodium silicate solutions, while 1.0mol/L hydrochloric acid solutions are added dropwise to maintain pH constant, after adding, insulation 0.5h, then the Ludox obtained in step (2) is added in above-mentioned bag silicon dispersion liquid and is incubated 0.5h, then by suspension mistake Filter and be washed with deionized the compound filter cake of zinc-titanium for the μ S/cm of filtrate electrical conductivity 134, obtaining coating processing.
4th, the preparation of water base zinc-titanium composite mortar：By the compound filter cake of zinc-titanium after the coating obtained in step (3) processing Again disperse in deionized water, the preservative Phenoxyethanol for adding 18.75g stirs (based on dispersion liquid quality), then Ground by sand mill and water base zinc-titanium composite mortar is made.
Comparative example 2
Under conditions of identical covering amount, coating process in step (3) in embodiment 1 is all used into Ludox in comparative example Coating process, for other operating conditions with embodiment 1, concrete operations are as described below：
1st, the preparation of zinc-titanium composite dispersion liquid：0.08kg wetting dispersing agent is added in 1.42kg deionized water PA25 stirs (based on powder quality), then adds 1kg zinc-titanium composite granule, stirs, it is adjusted with triethanolamine PH value is 9, obtains the compound pre-dispersed liquid of zinc-titanium, then grinds the compound pre-dispersed liquid of zinc-titanium by sand mill and zinc-titanium is made Composite dispersion liquid.
2nd, prepared by Ludox：Deionized water is warming up to 85 DEG C, its pH value is adjusted and is stirred for 10 while being added dropwise 0.8mol/L sodium silicate solution, while 1.0mol/L hydrochloric acid solution is added dropwise to maintain pH constant, during dropwise addition solution by Colourless is gradually that 0.3g/mL Ludox is standby into transparent light oyster white colloidal sol, obtained concentration.
3rd, coating is handled：Take obtained 0.3g/mL Ludox 0.584L stirrings in step (2) to be warming up to 85 DEG C, then will The zinc obtained in step (1)-titanium composite dispersion liquid, which is added under stirring in above-mentioned Ludox, is incubated 0.5h, then will suspend Liquid filters and is washed with deionized the compound filter cake of zinc-titanium for the μ S/cm of filtrate electrical conductivity 134, obtaining coating processing.
4th, the preparation of water base zinc-titanium composite mortar：By the compound filter cake of zinc-titanium after the coating obtained in step (3) processing Again disperse in deionized water, the preservative Phenoxyethanol for adding 18.75g stirs (based on dispersion liquid quality), then Ground by sand mill and water base zinc-titanium composite mortar is made.
Comparative example 3
Under conditions of identical covering amount, coating process in step (3) in embodiment 1 is all used into sodium metasilicate in comparative example Coating process, for other operating conditions with embodiment 1, concrete operations are as described below：
1st, the preparation of zinc-titanium composite dispersion liquid：0.08kg wetting dispersing agent is added in 1.42kg deionized water PA25 stirs (based on powder quality), then adds 1kg zinc-titanium composite granule, stirs, it is adjusted with triethanolamine PH value is 9, obtains the compound pre-dispersed liquid of zinc-titanium, then grinds the compound pre-dispersed liquid of zinc-titanium by sand mill and zinc-titanium is made Composite dispersion liquid.
2nd, coating is handled：The zinc obtained in step (1)-titanium composite dispersion liquid stirring is warming up to 85 DEG C, then while stirring Mix while 2.46L 0.8mol/L sodium silicate solutions are added dropwise, while 1.0mol/L hydrochloric acid solutions are added dropwise to maintain pH constant, add Afterwards, it is incubated 0.5h.Then suspension is filtered and is washed with deionized to the μ S/cm of filtrate electrical conductivity 134, obtained at coating The compound filter cake of zinc-titanium of reason.
3rd, the preparation of water base zinc-titanium composite mortar：By the compound filter cake of zinc-titanium after the coating obtained in step (2) processing Again disperse in deionized water, the preservative Phenoxyethanol for adding 18.75g stirs (based on dispersion liquid quality), then Ground by sand mill and water base zinc-titanium composite mortar is made.
Table 1 is dissolution test of the zinc ion in zinc-titanium composite mortar
The good and bad of coating effect is evaluated by detecting before and after coating in filtrate zinc ion concentration in the present invention, experimental result As shown in Table 1.Zinc ion dissolution phenomenon in zinc-titanium composite mortar can be significantly reduced by present invention process by table 1 is visible, And then more stable zinc-titanium composite mortar can be prepared and widen its application field.

Claims (8)

  1. A kind of 1. preparation method of water base zinc-titanium composite mortar, it is characterised in that：The preparation method processing step is as follows：
    (1), the preparation of zinc-titanium composite dispersion liquid：The wetting dispersing agent for adding powder gross mass 1~15% in deionized water stirs Mix uniformly, add zinc-titanium composite granule, stir, it is 8~10 to adjust dispersion liquid pH value with organic amine, and then grinding is Obtain zinc-titanium composite dispersion liquid；
    (2), prepared by Ludox：Deionized water is warming up to 75~95 DEG C, it is 8~10 to adjust its pH value, is stirred while dripping Add 0.1~1.5mol/L sodium silicate solution, while 0.1~2.0mol/L acid solution is added dropwise to maintain pH constant, be added dropwise During solution by colourless gradually into transparent light oyster white colloidal sol, it is standby；
    (3), coating is handled：It is molten that zinc titanium composite dispersion liquid in step (1) is added under stirring to the silicon that step (2) obtains In glue, 0.5~1h is incubated, is then stirred in 75~95 DEG C of temperature, pH value for 8~10 times while 0.1~1.5mol/ is added dropwise L sodium silicate solution, while the acid solution that 0.1~2.0mol/L is added dropwise maintains the pH constant, after adding, insulation 0.5~ 1h；Then suspension is filtered and is washed with deionized and to the μ S/cm of filtrate electrical conductivity≤200, obtain zinc-titanium of coating processing Compound filter cake；
    (4), the preparation of water base zinc-titanium composite mortar：The compound filter cake of zinc titanium after coating is handled will be obtained in step (3) again to divide Dissipate, the preservative for adding dispersion liquid quality 0.5~1% stirs, and then grinds and water base zinc-titanium composite mortar is made.
  2. 2. the preparation method of water base zinc-titanium composite mortar as claimed in claim 1, it is characterised in that：In the step (1) Wetting dispersing agent is：Polycarboxylate sodium's class, polycarboxylic acids ammonium salt class, Sodium Polyacrylate salt, one kind in polycarboxylic ethers or several Kind.
  3. 3. the preparation method of water base zinc-titanium composite mortar as claimed in claim 1, it is characterised in that：In the step (1) Organic amine is：One or more in triethanolamine, isopropanolamine, diisopropanolamine (DIPA).
  4. 4. the preparation method of water base zinc-titanium composite mortar as claimed in claim 1, it is characterised in that：In the step (2) The mass concentration of Ludox is 0.1~0.5g/mL.
  5. 5. the preparation method of water base zinc-titanium composite mortar as claimed in claim 1, it is characterised in that：The step (2) and step Suddenly the acid solution in (3) is：One kind or its mixed solution in hydrochloric acid, sulfuric acid, nitric acid.
  6. 6. the preparation method of water base zinc-titanium composite mortar as claimed in claim 1, it is characterised in that：Silicon in the step (3) The mass ratio of sour sodium and zinc-titanium composite granule is 0.05~0.3:1, the quality of the amount of sodium silicate and zinc-titanium composite granule Than with the oxide S iO of sodium metasilicate2Meter.
  7. 7. the preparation method of water base zinc-titanium composite mortar as claimed in claim 1, it is characterised in that：The step (1) and step Suddenly the milling apparatus in (4) is：One kind in sand mill, ball mill, ultrasonic cell disruptor.
  8. 8. the preparation method of water base zinc-titanium composite mortar as claimed in claim 1, it is characterised in that：In the step (4) Preservative is：One kind in benzoic acid and salt, sorbic acid and salt, Phenoxyethanol, sodium Diacetate, calcium propionate, sodium lactate.
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