CN107537290A - A kind of preparation method of compound-dehumidifying agent - Google Patents
A kind of preparation method of compound-dehumidifying agent Download PDFInfo
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- CN107537290A CN107537290A CN201710957058.9A CN201710957058A CN107537290A CN 107537290 A CN107537290 A CN 107537290A CN 201710957058 A CN201710957058 A CN 201710957058A CN 107537290 A CN107537290 A CN 107537290A
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Abstract
The invention belongs to air humidity to adjust field, and in particular to a kind of preparation method of compound-dehumidifying agent.The present invention is modified by using to vermiculite, improve the adsorption capacity and porosity of vermiculite, increase adsorbance, calcium chloride solution is immersed in after low-temperature treatment simultaneously, improve and adsorbance is carried out to calcium chloride, reuse freeze-drying, prevent the loss of calcium chloride, raw material is then used as using sodium metasilicate, Bio-sil is formed to wrap up modified vermiculite, recycle sodium acid carbonate increase porosity, organic silicon monomer is mixed in encapsulation process, make the polymerization of organic silicon monomer in the presence of catalyst, and form network structure in the hole of macroreticular resin, increase moisture absorption efficiency, and improve silica gel and the conjugation of PERFORMANCE OF MODIFIED VERMICULITE, the outflow of calcium chloride can effectively be suppressed simultaneously, and meet the chlorion of the calcium chloride release after water, the vermiculite being modified and silica gel absorption, prevent the corrosion to environment, and improve hygroscopic capacity.
Description
Technical field
The invention belongs to air humidity to adjust field, and in particular to a kind of preparation method of compound-dehumidifying agent.
Background technology
Dehumidizer is to use the solid with wet-out property or fluent material directly to be contacted with air, realizes removing for air
It is wet.Because with isothermal dehumidifying is easily achieved, irreversible loss is small, thermodynamics consummating degree is high;More low-grade heat can be used
Drive energy can be used as;It is simple in construction without larger moving component, it is easy to minimize;The dust in air, bacterium etc., which can be removed, to be had
Evil thing, improve air quality the advantages that and be used widely.Air humidity is one has close pass with people's life and production
The important environmental parameters of system, humidity have important meaning to human comfort, process of producing product, product quality and product storage life
Justice., can serious shadow if not being controlled to humidity especially in the production processes such as precision instrument, metrical instrument, electronics and chemical industry
Product quality, the precision of instrument and service life are rung, or even electronic product is not operated until scrapping.Article is in humidity
Deposited in environment, can due to mould erosion and moldy metamorphism;It can decline metal rusting, accuracy of instrument, insulation parameter reduction,
Great loss is caused to national economy.Air dewetting has been common problem, with the development of production and life water
Flat raising, air dewetting have developed and have formed a new technology.
Dehumidizer is divided into two kinds, and one kind is non-deliquescence dehumidizer, including silica gel, molecular sieve etc., another kind are deliquescence dehumidifying
Agent, such as hygroscopic salt, including calcium chloride, lithium chloride.Non- deliquescence dehumidizer, its moisture absorption mechanism is physical absorption, because it has
Big ratio surface and the capillary action containing substantial amounts of micropore produce the absorption to moisture.And deliquescence dehumidizer, such as moisture absorption
Property salt, including calcium chloride, lithium chloride.Its dominant mechanism is chemical absorbing, and moisture is absorbed by series of chemical.
Currently used dehumidizer has lithium chloride, silica gel, molecular sieve, calcium chloride etc..Although there is certain moisture sorption effect, there is also
Problem:The wettability powers such as calcium chloride, lithium chloride are strong, but it absorbs easily rupturable generation liquid after a large amount of water, and have severe corrosive,
Easily cause the corrosion of surrounding articles.Therefore, it is good and be not easily broken the dehumidizer of not corrosives to produce a kind of effect on moisture extraction
There is the very big market demand.
The content of the invention
The technical problems to be solved by the invention:For current dehumidizer after a large amount of water are absorbed easily rupturable generation liquid,
And caused liquid has corrosivity, the problem of causing the corrosion of surrounding articles, the invention provides a kind of compound-dehumidifying agent
Preparation method.
In order to solve the above technical problems, the present invention is using technical scheme as described below:
A kind of preparation method of compound-dehumidifying agent, the preparation method comprise the following steps:
(1)Take vermiculite to be put into calcining furnace to be calcined, crush, sieving, collect sieving particle, by sieving particle, tricresyl phosphate second
Ester and cetyl trimethylammonium bromide, which are put into ball mill, carries out ball milling, collects ball milling thing;
(2)Ball milling thing is placed at -10~-5 DEG C and carries out freezing processing, places into 40~50 DEG C of calcium chloride solutions and soaks, it is cold
It is lyophilized dry, collect dried object;
(3)Count in parts by weight, take 80~85 parts of water, 45~50 parts of dimethylbenzene, 32~36 parts of sodium metasilicate, 23~27 parts of dryings
Thing, 13~16 parts of triethyl group amino silanes, 11~15 parts of hexamethyldisilanes, 10~19 parts of ammonium chloride solutions, 8~13 parts of carbonic acid
Hydrogen sodium, 4~6 parts of surfactants and 2~5 parts of catalyst;
(4)Water, dimethylbenzene, sodium metasilicate, dried object and surfactant are put into reactor first, protected using nitrogen,
Preheated at 40~50 DEG C, then add triethyl group amino silane, hexamethyldisilane and catalyst, be warming up to 92~96 DEG C, stir
40~43min is mixed, then ammonium chloride solution is added dropwise, after being added dropwise to complete, cooling, sodium acid carbonate is added, discharging, collects out material,
It is spray-dried, collects dried object, produce dehumidizer.
The step(1)Middle sieving particle, the mass ratio of triethyl phosphate and cetyl trimethylammonium bromide for 8~
10:2:1。
The surfactant is appointing in dodecyldimethylammonium hydroxide inner salt, dodecyl Hydroxypropyl phosphate ester glycine betaine
Meaning is a kind of.
The catalyst is any one in sodium hydroxide solution, potassium hydroxide solution.
Compared with other method, advantageous effects are the present invention:The present invention is modified by using to vermiculite, improves vermiculite
Adsorption capacity and porosity, increase adsorbance, while calcium chloride solution be immersed in after low-temperature treatment, improve and calcium chloride is entered
Row adsorbance, freeze-drying is reused, prevent the loss of calcium chloride, then using sodium metasilicate as raw material, form Bio-sil pair
Modified vermiculite is wrapped up, and recycles sodium acid carbonate increase porosity, organic silicon monomer is mixed in encapsulation process, is being urged
Make the polymerization of organic silicon monomer in the presence of agent, and network structure formed in the hole of macroreticular resin, increase moisture absorption efficiency,
And silica gel and the conjugation of PERFORMANCE OF MODIFIED VERMICULITE are improved, while can effectively suppress the outflow of calcium chloride, and meet the chlorination after water
The chlorion of calcium release, the vermiculite being modified and silica gel absorption, it is therefore prevented that the corrosion to environment, and improve hygroscopic capacity.
Embodiment
The selection of surfactant is dodecyldimethylammonium hydroxide inner salt, in dodecyl Hydroxypropyl phosphate ester glycine betaine
Any one.
The selection of catalyst is any one in 1.3mol/L sodium hydroxide solutions, 1.1mol/L potassium hydroxide solutions.
A kind of preparation method of compound-dehumidifying agent, the preparation method comprise the following steps:
(1)Take vermiculite to be put into calcining furnace, calcining 50min is carried out at 1000~1200 DEG C, crush, cross 200 mesh sieves, collected
Particle is sieved, is in mass ratio 8~10:2:1, sieving particle, triethyl phosphate and cetyl trimethylammonium bromide are put into ball
In grinding machine, 30~40min of ball milling is carried out with 800r/min, collects ball milling thing;
(2)Ball milling thing is placed at -10~-5 DEG C progress 1~2h of freezing processing, place into 6~8 times of ball milling amount of substance 40~
45~55min is soaked in 50 DEG C of 1.6mol/L calcium chloride solutions, freeze-drying, collects dried object;
(3)Count in parts by weight, take 80~85 parts of water, 45~50 parts of dimethylbenzene, 32~36 parts of sodium metasilicate, 23~27 parts of dryings
Thing, 13~16 parts of triethyl group amino silanes, 11~15 parts of hexamethyldisilanes, 10~19 parts of ammonium chloride solutions, 8~13 parts of carbonic acid
Hydrogen sodium, 4~6 parts of surfactants and 2~5 parts of catalyst;
(4)Water, dimethylbenzene, sodium metasilicate, dried object and surfactant are put into reactor first, protected using nitrogen,
30~40min is preheated at 40~50 DEG C, triethyl group amino silane, hexamethyldisilane and catalyst is then added, is warming up to 92
~96 DEG C, 40~43min is stirred, then ammonium chloride solution is added dropwise with 1mL/s, after being added dropwise to complete, room temperature is cooled to, adds carbonic acid
Hydrogen sodium, 30min is stirred, discharging, material is collected out, is spray-dried, dried object is collected, produces dehumidizer.
Example 1
The selection of surfactant is dodecyldimethylammonium hydroxide inner salt.
The selection of catalyst is 1.1mol/L potassium hydroxide solutions.
A kind of preparation method of compound-dehumidifying agent, the preparation method comprise the following steps:
(1)Take vermiculite to be put into calcining furnace, calcining 50min is carried out at 1150 DEG C, crush, cross 200 mesh sieves, collect sieving
Grain, is in mass ratio 89:2:1, sieving particle, triethyl phosphate and cetyl trimethylammonium bromide are put into ball mill,
Ball milling 35min is carried out with 800r/min, collects ball milling thing;
(2)Ball milling thing is placed in progress freezing processing 1.5h at -8 DEG C, places into 45 DEG C of 1.6mol/L chlorine of 7 times of ball milling amount of substance
Change in calcium solution and soak 50min, be freeze-dried, collect dried object;
(3)Count in parts by weight, take 83 parts of water, 48 parts of dimethylbenzene, 34 parts of sodium metasilicate, 25 parts of dried objects, 15 parts of triethyl group amino
Silane, 13 parts of hexamethyldisilanes, 14 parts of ammonium chloride solutions, 10 parts of sodium acid carbonates, 5 parts of surfactants and 3 parts of catalyst;
(4)Water, dimethylbenzene, sodium metasilicate, dried object and surfactant are put into reactor first, protected using nitrogen,
35min is preheated at 45 DEG C, then adds triethyl group amino silane, hexamethyldisilane and catalyst, is warming up to 94 DEG C, stirring
41min, then ammonium chloride solution is added dropwise with 1mL/s, after being added dropwise to complete, room temperature is cooled to, adds sodium acid carbonate, stirs 30min,
Discharging, collects out material, is spray-dried, and collects dried object, produces dehumidizer.
Example 2
The selection of surfactant is dodecyl Hydroxypropyl phosphate ester glycine betaine.
The selection of catalyst is 1.1mol/L potassium hydroxide solutions.
A kind of preparation method of compound-dehumidifying agent, the preparation method comprise the following steps:
(1)Take vermiculite to be put into calcining furnace, calcining 50min is carried out at 1200 DEG C, crush, cross 200 mesh sieves, collect sieving
Grain, is in mass ratio 10:2:1, sieving particle, triethyl phosphate and cetyl trimethylammonium bromide are put into ball mill,
Ball milling 40min is carried out with 800r/min, collects ball milling thing;
(2)Ball milling thing is placed in progress freezing processing 2h at -5 DEG C, places into 50 DEG C of 1.6mol/L chlorinations of 8 times of ball milling amount of substance
55min is soaked in calcium solution, is freeze-dried, collects dried object;
(3)Count in parts by weight, take 85 parts of water, 50 parts of dimethylbenzene, 36 parts of sodium metasilicate, 27 parts of dried objects, 16 parts of triethyl group amino
Silane, 15 parts of hexamethyldisilanes, 19 parts of ammonium chloride solutions, 13 parts of sodium acid carbonates, 6 parts of surfactants and 5 parts of catalyst;
(4)Water, dimethylbenzene, sodium metasilicate, dried object and surfactant are put into reactor first, protected using nitrogen,
40min is preheated at 50 DEG C, then adds triethyl group amino silane, hexamethyldisilane and catalyst, is warming up to 96 DEG C, stirring
43min, then ammonium chloride solution is added dropwise with 1mL/s, after being added dropwise to complete, room temperature is cooled to, adds sodium acid carbonate, stirs 30min,
Discharging, collects out material, is spray-dried, and collects dried object, produces dehumidizer.
Example 3
The selection of surfactant is dodecyldimethylammonium hydroxide inner salt.
The selection of catalyst is 1.3mol/L sodium hydroxide solutions.
A kind of preparation method of compound-dehumidifying agent, the preparation method comprise the following steps:
(1)Take vermiculite to be put into calcining furnace, calcining 50min is carried out at 1000 DEG C, crush, cross 200 mesh sieves, collect sieving
Grain, is in mass ratio 8:2:1, sieving particle, triethyl phosphate and cetyl trimethylammonium bromide are put into ball mill, with
800r/min carries out ball milling 30min, collects ball milling thing;
(2)Ball milling thing is placed in progress freezing processing 1h at -10 DEG C, places into 40 DEG C of 1.6mol/L chlorine of 6 times of ball milling amount of substance
Change in calcium solution and soak 45min, be freeze-dried, collect dried object;
(3)Count in parts by weight, take 80 parts of water, 45 parts of dimethylbenzene, 32 parts of sodium metasilicate, 23 parts of dried objects, 13 parts of triethyl group amino
Silane, 11 parts of hexamethyldisilanes, 10 parts of ammonium chloride solutions, 8 parts of sodium acid carbonates, 4 parts of surfactants and 2 parts of catalyst;
(4)Water, dimethylbenzene, sodium metasilicate, dried object and surfactant are put into reactor first, protected using nitrogen,
30min is preheated at 40 DEG C, then adds triethyl group amino silane, hexamethyldisilane and catalyst, is warming up to 92 DEG C, stirring
40min, then ammonium chloride solution is added dropwise with 1mL/s, after being added dropwise to complete, room temperature is cooled to, adds sodium acid carbonate, stirs 30min,
Discharging, collects out material, is spray-dried, and collects dried object, produces dehumidizer.
Reference examples:The dehumidizer of company of Jining City production.
The dehumidizer of dehumidizer obtained by examples detailed above and reference examples is detected, specific detection is as follows:
Under conditions of the dehumidizer of dehumidizer obtained by example and reference examples is placed on into 25 DEG C and 80%RH respectively, put by dehumidizer
10 × 10cm plank is put, its hygroscopic capacity is tested after one month and observes packaging bag rupture and plank corrosion condition.Test result
It is shown in Table 1.
Table 1:
Test event | Example 1 | Example 2 | Example 3 | Reference examples |
Hygroscopic capacity(g) | 251 | 223 | 221 | 158~179 |
Packaging bag rupture event | Crack-free | Crack-free | Crack-free | Rupture |
Plank corrosion condition | Do not corrode | Do not corrode | Do not corrode | Moderate corrosion, corrode to plank |
Summary, dehumidizer hygroscopic capacity of the invention is big and is not easily broken and causes to corrode, and is worth promoting.
Claims (4)
1. a kind of preparation method of compound-dehumidifying agent, it is characterised in that the preparation method comprises the following steps:
(1)Take vermiculite to be put into calcining furnace to be calcined, crush, sieving, collect sieving particle, by sieving particle, tricresyl phosphate second
Ester and cetyl trimethylammonium bromide, which are put into ball mill, carries out ball milling, collects ball milling thing;
(2)Ball milling thing is placed at -10~-5 DEG C and carries out freezing processing, places into 40~50 DEG C of calcium chloride solutions and soaks, it is cold
It is lyophilized dry, collect dried object;
(3)Count in parts by weight, take 80~85 parts of water, 45~50 parts of dimethylbenzene, 32~36 parts of sodium metasilicate, 23~27 parts of dryings
Thing, 13~16 parts of triethyl group amino silanes, 11~15 parts of hexamethyldisilanes, 10~19 parts of ammonium chloride solutions, 8~13 parts of carbonic acid
Hydrogen sodium, 4~6 parts of surfactants and 2~5 parts of catalyst;
(4)Water, dimethylbenzene, sodium metasilicate, dried object and surfactant are put into reactor first, protected using nitrogen,
Preheated at 40~50 DEG C, then add triethyl group amino silane, hexamethyldisilane and catalyst, be warming up to 92~96 DEG C, stir
40~43min is mixed, then ammonium chloride solution is added dropwise, after being added dropwise to complete, cooling, sodium acid carbonate is added, discharging, collects out material,
It is spray-dried, collects dried object, produce dehumidizer.
2. the preparation method of compound-dehumidifying agent according to claim 1, it is characterised in that the step(1)Middle sieving
The mass ratio of grain, triethyl phosphate and cetyl trimethylammonium bromide is 8~10:2:1.
3. the preparation method of compound-dehumidifying agent according to claim 1, it is characterised in that the surfactant is 12
Any one in alkyl dimethyl betaine, dodecyl Hydroxypropyl phosphate ester glycine betaine.
4. the preparation method of compound-dehumidifying agent according to claim 1, it is characterised in that the catalyst is sodium hydroxide
Any one in solution, potassium hydroxide solution.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN108892486A (en) * | 2018-08-23 | 2018-11-27 | 安徽瑞泰新材料科技有限公司 | A kind of anti-explosion refractory castable |
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CN101850983A (en) * | 2010-03-12 | 2010-10-06 | 中国科学院新疆理化技术研究所 | Ball milling method for preparing organic vermiculite with large layer distance |
CN105561915A (en) * | 2016-01-29 | 2016-05-11 | 袁一军 | Novel dehumidifying agent and making method thereof |
CN106345242A (en) * | 2016-10-28 | 2017-01-25 | 广西大学 | Dehumidifying agent for removing water from air and preparation method thereof |
CN107051375A (en) * | 2017-03-24 | 2017-08-18 | 佛山市南海依泰科空气处理设备有限公司 | A kind of desiccant wheel and preparation method thereof |
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2017
- 2017-10-16 CN CN201710957058.9A patent/CN107537290A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
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WO1999012641A1 (en) * | 1997-09-08 | 1999-03-18 | Inalfa Industries B.V. | Desiccant |
CN101850983A (en) * | 2010-03-12 | 2010-10-06 | 中国科学院新疆理化技术研究所 | Ball milling method for preparing organic vermiculite with large layer distance |
CN105561915A (en) * | 2016-01-29 | 2016-05-11 | 袁一军 | Novel dehumidifying agent and making method thereof |
CN106345242A (en) * | 2016-10-28 | 2017-01-25 | 广西大学 | Dehumidifying agent for removing water from air and preparation method thereof |
CN107051375A (en) * | 2017-03-24 | 2017-08-18 | 佛山市南海依泰科空气处理设备有限公司 | A kind of desiccant wheel and preparation method thereof |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN108892486A (en) * | 2018-08-23 | 2018-11-27 | 安徽瑞泰新材料科技有限公司 | A kind of anti-explosion refractory castable |
CN108892486B (en) * | 2018-08-23 | 2021-06-04 | 安徽瑞泰新材料科技有限公司 | Explosion-proof castable |
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