CN106753322A - A kind of synthetic method of thermochromic material - Google Patents
A kind of synthetic method of thermochromic material Download PDFInfo
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- CN106753322A CN106753322A CN201710023209.3A CN201710023209A CN106753322A CN 106753322 A CN106753322 A CN 106753322A CN 201710023209 A CN201710023209 A CN 201710023209A CN 106753322 A CN106753322 A CN 106753322A
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- China
- Prior art keywords
- thermochromic material
- solution
- thermochromic
- synthetic method
- crystallization
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- 239000000463 material Substances 0.000 title claims abstract description 30
- 238000010189 synthetic method Methods 0.000 title claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 150000001875 compounds Chemical class 0.000 claims abstract description 8
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical class [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims abstract description 8
- VLAPMBHFAWRUQP-UHFFFAOYSA-L molybdic acid Chemical compound O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 0.000 claims abstract description 7
- NASFKTWZWDYFER-UHFFFAOYSA-N sodium;hydrate Chemical compound O.[Na] NASFKTWZWDYFER-UHFFFAOYSA-N 0.000 claims abstract description 7
- QIJRTFXNRTXDIP-UHFFFAOYSA-N (1-carboxy-2-sulfanylethyl)azanium;chloride;hydrate Chemical compound O.Cl.SCC(N)C(O)=O QIJRTFXNRTXDIP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229960001305 cysteine hydrochloride Drugs 0.000 claims abstract description 5
- 239000013078 crystal Substances 0.000 claims description 11
- 238000002425 crystallisation Methods 0.000 claims description 11
- 230000008025 crystallization Effects 0.000 claims description 11
- 239000012153 distilled water Substances 0.000 claims description 11
- 239000013067 intermediate product Substances 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000007792 addition Methods 0.000 claims description 3
- 238000013019 agitation Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 3
- 238000000967 suction filtration Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 2
- 238000004821 distillation Methods 0.000 claims 1
- 238000005406 washing Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 5
- GFHNAMRJFCEERV-UHFFFAOYSA-L cobalt chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Co+2] GFHNAMRJFCEERV-UHFFFAOYSA-L 0.000 abstract description 3
- 238000007639 printing Methods 0.000 abstract description 3
- 230000002441 reversible effect Effects 0.000 abstract description 3
- 239000004753 textile Substances 0.000 abstract description 3
- 239000002253 acid Substances 0.000 abstract description 2
- 238000005034 decoration Methods 0.000 abstract description 2
- 230000008569 process Effects 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 abstract description 2
- LJPYJRMMPVFEKR-UHFFFAOYSA-N prop-2-ynylurea Chemical compound NC(=O)NCC#C LJPYJRMMPVFEKR-UHFFFAOYSA-N 0.000 abstract 1
- 239000000047 product Substances 0.000 description 4
- 238000011160 research Methods 0.000 description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- -1 molybdenum sulphur organic compound Chemical class 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 230000006386 memory function Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 150000002902 organometallic compounds Chemical class 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K9/00—Tenebrescent materials, i.e. materials for which the range of wavelengths for energy absorption is changed as a result of excitation by some form of energy
- C09K9/02—Organic tenebrescent materials
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F15/00—Compounds containing elements of Groups 8, 9, 10 or 18 of the Periodic Table
- C07F15/06—Cobalt compounds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2211/00—Chemical nature of organic luminescent or tenebrescent compounds
- C09K2211/18—Metal complexes
- C09K2211/187—Metal complexes of the iron group metals, i.e. Fe, Co or Ni
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
Abstract
The invention discloses a kind of synthetic method of thermochromic material, by two molybdic acid hydrate sodium, cobalt chloride hexahydrate, L-cysteine hydrochloride monohydrate (cys), the component mixed preparing such as nine hydrated sodium sulfides is formed for the invention.The present invention uses cysteine hydrochloride, two molybdic acid hydrate sodium, nine hydrated sodium sulfides are primary raw material first synthetic mesophase product in acid condition, afterwards with cobalt chloride hexahydrate reaction generation thermochromic material, product shows the material for crystalline state through analysis result, non-indefiniteness compound；TG is analyzed and thermochromic properties test result illustrates that this kind of material has thermochromic properties, 50 DEG C of discoloring temperature, and color is reducible under water ambient conditions, and process is reversible.Thermochromic material method prepared by the present invention is simple and easy to control, and product purity is high, and product can be widely used in the fields such as textile industry, military field, ink printing, anti-fake mark, daily decoration and Aero-Space.
Description
Technical field
The present invention relates to field of new, and in particular to a kind of synthetic method of thermochromic material.
Background technology
Thermochromic material typically refer to a class compound or mixture be heated or cooling condition under color change,
And have hot memory function and can be with the intelligent material of Reusability.This class material is widely used in textile industry, military neck
The fields such as domain, ink printing, anti-fake mark, daily decoration and Aero-Space.
Thermochromic material has the research history in more than halfth century abroad, and has been developed that liquid crystal, nothing up to now
Numerous materials with property such as machine, Organic and polymer materials and large biological molecule.Research compared to China in this field rises
In step slightly evening, the material category developed is also relatively simple with quantity.Molybdenum system organo-metallic compound is that transition metal organises
The important research field learned, particularly molybdenum sulphur organic compound.Its synthesis, structure and application study are very active always
And many molybdenum system organic compounds have reversible thermochromic characteristic.
The content of the invention
Present invention aim at, there is provided a kind of synthetic method of the thermochromic material of high comprehensive performance, the present invention is adopted
Technical scheme is as follows：
A kind of synthetic method of thermochromic material, it is characterised in that be prepared from by following steps：
（1）Weigh during two molybdic acid hydrate sodium and nine hydrated sodium sulfides add distilled water, then measure during concentrated hydrochloric acid adds solution, then
By the solution heating stirring to 90-92 DEG C and constant temperature 20-30min until solution is in orange red；
（2）Weigh the cysteine hydrochloride monohydrates of L mono- and add step（1）Solution in, keep the temperature at 90-92 DEG C,
Stirring is concentrated into volume and is reduced to 40-50mL, orange crystal occurs, solution is stored in together with crystal after being stood in refrigerator and taken out
Suction filtration, drying at room temperature after scrubbed crystallization, that is, obtain intermediate product；
（3）By step（2）The intermediate product crystal of middle gained is dissolved in the distilled water of heat, then weighs CoC12·6H2O is dissolved in steaming
In distilled water, two kinds of solution are mixed under agitation, stop heating after dissolving immediately, yellow is slowly separated out after natural cooling difficult
Molten lenticular compound, filtering, after dry under room temperature condition after scrubbed crystallization, you can obtain thermochromic material.
Further, the step（1）In two molybdic acid hydrate sodium and the ratio between nine hydrated sodium sulfide additions be 1:2.
Further, the step（2）Middle wash crystallization is to use distilled water and each wash crystallization chemical combination of absolute ethyl alcohol respectively
Thing 2-3 times.
Further, described step（3）The intermediate product crystal and CoC1 of middle addition2·6H2O is according to identical material
Amount.
The present invention is relative to the beneficial effect of prior art：The present invention uses cysteine hydrochloride, two molybdic acid hydrates
Sodium, nine hydrated sodium sulfides are primary raw material first synthetic mesophase product in acid condition, reacted with cobalt chloride hexahydrate generate afterwards
Thermochromic material, and its structure and property have carried out performance test analysis, analysis result shows the material for crystalline state, non-nothing
Qualitative compound；TG is analyzed and thermochromic properties test result illustrates that this kind of material has thermochromic properties, color temperature
50 DEG C of degree, and color is reducible under water ambient conditions, process is reversible.Thermochromic material method prepared by the present invention is simple
Easy to control, product purity is high, and product can be widely used in textile industry, military field, ink printing, anti-fake mark, daily dress
It is decorated with and the field such as Aero-Space.
Specific embodiment
Design of the invention and the technique effect for producing are clearly and completely described below with reference to embodiment, with
It is completely understood by the purpose of the present invention, feature and effect.Obviously, described embodiment is that a part of the invention is implemented
Example, rather than whole embodiments, based on embodiments of the invention, those skilled in the art is not before creative work is paid
Obtained other embodiment is put, the scope of protection of the invention is belonged to.
Embodiment 1：A kind of synthetic method of thermochromic material, is prepared from by following steps：
（1）Weigh during two molybdic acid hydrate sodium 5g and nine hydrated sodium sulfide 10g add distilled water, then measure concentrated hydrochloric acid 5ml add it is molten
In liquid, then by the solution heating stirring to 90-92 DEG C and constant temperature 20-30min until solution is in orange red；
（2）Weigh the cysteine hydrochloride monohydrate 6g of L mono- and add step（1）Solution in, keep the temperature at 90-92
DEG C, stirring is concentrated into volume and is reduced to 40-50mL, orange crystal occurs, solution is stored in together with crystal after being stood in refrigerator
Suction filtration is taken out, respectively with distilled water and each wash crystallization compound of absolute ethyl alcohol 2-3 times, drying at room temperature after crystallization, that is, in obtaining
Between product；
（3）By step（2）The intermediate product crystal 0.5mol of middle gained is dissolved in the distilled water of heat, then is weighed
0.5molCoC12·6H2O is dissolved in distilled water, and two kinds of solution are mixed under agitation, stops heating after dissolving immediately, from
Yellow indissoluble lenticular compound is slowly so separated out after cooling, is filtered, after dry under room temperature condition after scrubbed crystallization, you can
Obtain thermochromic material.
Better embodiment of the invention is illustrated above, but the invention is not limited to the implementation
Example, those of ordinary skill in the art can also make a variety of equivalent modifications or replace on the premise of without prejudice to spirit of the invention
Change, these equivalent modifications or replacement are all contained in the application claim limited range.
Claims (4)
1. a kind of synthetic method of thermochromic material, it is characterised in that be prepared from by following steps：
（1）Weigh during two molybdic acid hydrate sodium and nine hydrated sodium sulfides add distilled water, then measure during concentrated hydrochloric acid adds solution, then
By the solution heating stirring to 90-92 DEG C and constant temperature 20-30min until solution is in orange red；
（2）Weigh the cysteine hydrochloride monohydrates of L mono- and add step（1）Solution in, keep the temperature at 90-92 DEG C,
Stirring is concentrated into volume and is reduced to 40-50mL, orange crystal occurs, solution is stored in together with crystal after being stood in refrigerator and taken out
Suction filtration, drying at room temperature after scrubbed crystallization, that is, obtain intermediate product；
（3）By step（2）The intermediate product crystal of middle gained is dissolved in the distilled water of heat, then weighs CoC12·6H2O is dissolved in distillation
In water, two kinds of solution are mixed under agitation, stop heating after dissolving immediately, yellow indissoluble is slowly separated out after natural cooling
Lenticular compound, filtering, after dry under room temperature condition after scrubbed crystallization, you can obtain thermochromic material.
2. the synthetic method of thermochromic material according to claim 1, it is characterised in that the step（1）In two
The ratio between molybdic acid hydrate sodium and nine hydrated sodium sulfide additions are 1:2.
3. the synthetic method of thermochromic material according to claim 1, it is characterised in that the step（2）Middle washing
Crystallization is respectively with distilled water and each wash crystallization compound of absolute ethyl alcohol 2-3 times.
4. the synthetic method of thermochromic material according to claim 1, it is characterised in that described step（3）In add
Plus intermediate product crystal and CoC12·6H2O according to identical material amount.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710023209.3A CN106753322A (en) | 2017-01-13 | 2017-01-13 | A kind of synthetic method of thermochromic material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710023209.3A CN106753322A (en) | 2017-01-13 | 2017-01-13 | A kind of synthetic method of thermochromic material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106753322A true CN106753322A (en) | 2017-05-31 |
Family
ID=58948281
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710023209.3A Withdrawn CN106753322A (en) | 2017-01-13 | 2017-01-13 | A kind of synthetic method of thermochromic material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106753322A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112608730B (en) * | 2020-11-30 | 2023-01-20 | 天津孚信阳光科技有限公司 | One-way color-changing nano material and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57123283A (en) * | 1981-01-23 | 1982-07-31 | Pilot Ink Co Ltd | Thermochromic material |
| CN1671816A (en) * | 2001-05-15 | 2005-09-21 | 欧罗克拉公司 | Thermochromic material |
-
2017
- 2017-01-13 CN CN201710023209.3A patent/CN106753322A/en not_active Withdrawn
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57123283A (en) * | 1981-01-23 | 1982-07-31 | Pilot Ink Co Ltd | Thermochromic material |
| CN1671816A (en) * | 2001-05-15 | 2005-09-21 | 欧罗克拉公司 | Thermochromic material |
Non-Patent Citations (1)
| Title |
|---|
| 姚媛媛等: "钼基有机配合物热致变色材料的合成", 《山东化工》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112608730B (en) * | 2020-11-30 | 2023-01-20 | 天津孚信阳光科技有限公司 | One-way color-changing nano material and preparation method and application thereof |
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| PB01 | Publication | ||
| PB01 | Publication | ||
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| SE01 | Entry into force of request for substantive examination | ||
| WW01 | Invention patent application withdrawn after publication | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20170531 |