CN1238719C - Humidity chromogenic indicator and chromatropic silica gel prepared therwith and its preparing method - Google Patents
Humidity chromogenic indicator and chromatropic silica gel prepared therwith and its preparing method Download PDFInfo
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- CN1238719C CN1238719C CN 02127021 CN02127021A CN1238719C CN 1238719 C CN1238719 C CN 1238719C CN 02127021 CN02127021 CN 02127021 CN 02127021 A CN02127021 A CN 02127021A CN 1238719 C CN1238719 C CN 1238719C
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Abstract
The present invention provides a humidity chromogenic indicator for color changing silica gel, which contains organic solvents, 10 to 40 wt% of inorganic salt and 0.1 to 5 wt% of chrominance indicator, and the humidity chromogenic indicator does not contain cobalt. Because the humidity chromogenic indicator of the present invention does not contain cobalt or other valuable radioactive elements, the pollution to the environment and the harm to human bodies are thoroughly eliminated; therefore, the humidity chromogenic indicator is a good product with environmental protection. In addition, the cost of the indicator of the present invention is low, and the color changing silica gel prepared by the indicator can be recycled.
Description
Technical field
This product relates to a kind of silica gel with the colourity indicator and with the discolour silica gel and the preparation method of its preparation.More particularly, relate to a kind of discolour silica gel humidity chromogenic indicator, and with discolour silica gel of its production and preparation method thereof.
Background technology
Discolour silica gel normally is that raw material is contaminated cobalt chloride (CoCl with silica gel
26H
2O) blue glue and the discolour silica gel made are partly mixed in drying agent during use, utilize its moisture absorption variable color to reach the purpose that shows or detect entire environment humidity, the repeated use of can also regenerating simultaneously.Because the developer that discolour silica gel adopted mostly is the cobalt chloride (CoCl of band water of crystallization
26H
2O), on the one hand, big and its isotope Co of its toxicity
60Have radioactivity, therefore bigger to human body harm, on the other hand, cobalt is valuable rare metal, causes the cost of discolour silica gel high.Therefore press for the cold substitute of a kind of non-toxic inexpensive.
Summary of the invention
One object of the present invention just provides a kind of like this humidity chromogenic indicator of producing cheapness that discolour silica gel uses, nontoxic, environmentally safe.
A further object of the present invention provides a kind of like this discolour silica gel, and this discolour silica gel has used humidity chromogenic indicator of the present invention.
Another purpose of the present invention provides a kind of preparation method of discolour silica gel of the present invention.
Summary of the invention
The inventor has succeeded in developing a kind of NEW TYPE OF COMPOSITE humidity chromogenic indicator at above-mentioned requirements, and it does not contain valuable radioelement such as cobalt, thereby has thoroughly eliminated to the pollution of environment and to the harm of human body, is a kind of good environment-friendly products.In addition, because indicator of the present invention has adopted cheap raw material, therefore with low cost.And, the discolour silica gel that makes by this indicator use of can repeatedly regenerating.
The invention provides a kind of discolour silica gel humidity chromogenic indicator, it contains organic solvent, in the general assembly (TW) of final indicator, the colourity indicator of the inorganic salts of 10-40wt% and 0.1-5wt%, and be substantially free of cobalt.
The present invention also provides a kind of discolour silica gel, it contains the inorganic salts of 0.1-4.5wt%, the colourity indicator of 0.01-0.03wt%, the organic dyestuff of 0.001-0.01wt% and as the granular colloidal silica with nano micropore structure capable of surplus, and be substantially free of cobalt.
In addition, the present invention also provides a kind of preparation method of discolour silica gel, comprises the steps:
(a) moisture absorption has nanometer level microporous Kiselgel A, moisture absorption to be put in do not burst in the tap water till;
(b) will contaminate in advance in the immersion of the Kiselgel A after the moisture absorption organic dyestuff solution, the preferred pre-dip-dye time is 1-1.5 hour;
(c) will immerse through the silica gel of pre-dip-dye in the humidity chromogenic indicator solution of the present invention and contaminate, take out dry then.
Detailed description of the preferred embodiments
The invention provides a kind of discolour silica gel indicator, it contains organic solvent, in the general assembly (TW) of final indicator, the colourity indicator of the inorganic salts of 10-40wt% and 0.1-5wt%, and be substantially free of cobalt.
Be applicable to that representative examples of organic of the present invention includes but not limited to absolute ethyl alcohol, 95% ethanol, ethylene glycol, glycerine, isopropyl alcohol, one or more in the n-propanol equal solvent are more preferably used absolute ethyl alcohol, ethylene glycol and 95% ethanol.
The example that is applicable to the inorganic salts of humidity chromogenic indicator of the present invention includes, but not limited to ferric trichloride, ferrous sulphate, iron sulfate (III) ammonium, potassium permanganate, copper sulphate etc. and their potpourri.Wherein, preferred ferric trichloride, iron sulfate (III) ammonium, potassium permanganate or two or more potpourri wherein, concrete consumption is decided on the colourity situation of change.
Various inorganic salts are preferably 10%-40% at discolour silica gel with the total weight percent content in the indicator among the present invention, more preferably 10-30%.According to a kind of preferred embodiment, discolour silica gel is with containing 0-30wt% ferric trichloride, 0-40wt% iron sulfate (III) ammonium, 0-1wt% copper sulphate, the potassium permanganate of 0-5wt% and the ferrous sulphate of 0-30wt% in the indicator.
Discolour silica gel of the present invention is meant a kind of reagent of indicating different colours along with the variation of environmental physics variation and electrochemical conditions with various colourity indicator contained in the humidity chromogenic indicator, and it is used for showing the color of different humidity.The example that is applicable to colourity indicator of the present invention includes but not limited to phenolphthalein, reindeer moss, bromine phenols dyestuff, thymol blue, methyl red, orange N and two or more potpourri wherein.Various colourity indicator are preferably 0-5wt% at discolour silica gel with the total weight percent content in the indicator.
Humidity chromogenic indicator of the present invention can adopt following method preparation: at first, the colourity indicator is dissolved in the organic solution that makes the colourity indicator among the suitable organic solvent, and inorganic salts are dissolved in the water make inorganic salt solution, then two kinds of solution are mixed according to predetermined ratio.In the potpourri, the ratio of water and organic solvent is not particularly limited, but preferably based on organic solvent, the consumption of water may be as few as to be enough to inorganic salts are dissolved just.Promptly get humidity chromogenic indicator by above-mentioned steps.The concentration of inorganic salt solution is preferably 10%～45%.Also can directly colourity indicator and inorganic salt solution be joined in the organic solvent, stirring and dissolving makes mixed solution.
The present invention also provides a kind of discolour silica gel, it contains the inorganic salts of 0.1-4.5wt%, the colourity indicator of 0.01-0.03wt%, the organic dyestuff of 0.001-0.01wt% and as the granular colloidal silica with nano micropore structure capable of surplus, and be substantially free of cobalt.
The preferred average pore size of granular colloidal silica that is applicable to discolour silica gel of the present invention is 10-50 , more preferably the Kiselgel A of 20-30 , the U.S. high chemical industry company limited production of preferred especially Qingdao and the serial Kiselgel A of selling.
The example that is applicable to the inorganic salts of discolour silica gel of the present invention includes, but not limited to ferric trichloride, ferrous sulphate, iron sulfate (III) ammonium, potassium permanganate, copper sulphate etc. and their potpourri.Wherein, preferred ferric trichloride, iron sulfate (III) ammonium, potassium permanganate or its potpourri, concrete consumption is decided on the colourity situation of change.
The various colourity indicator that are applicable to discolour silica gel of the present invention are used for showing the color of different humidity, and the example includes but not limited to phenolphthalein, reindeer moss, bromine phenols dyestuff, thymol blue, methyl red, orange N and their potpourri.
The organic dyestuff except that above-mentioned colourity indicator that is applicable to discolour silica gel of the present invention plays auxiliary colour developing effect, and the example includes but not limited to polar yellow GN, Acid Light Yellow G, acid brilliant yellow 2g, acid scarlet, alkaline pink, gentian violet and composition thereof.
The present invention also provides a kind of method for preparing discolour silica gel, comprises the steps:
(a) moisture absorption has nanometer level microporous Kiselgel A, moisture absorption to be put in do not burst in the tap water till;
(b) will contaminate in advance in the immersion of the Kiselgel A after the moisture absorption organic dyestuff solution, the preferred pre-dip-dye time is 1-1.5 hour;
(c) will immerse through the silica gel of pre-dip-dye in the humidity chromogenic indicator solution of the present invention and contaminate, take out dry then.
The organic dyestuff that uses in the above-mentioned steps (b) is preferably from polar yellow GN, Acid Light Yellow G, acid brilliant yellow 2g, acid scarlet, alkaline pink, gentian violet and two or more potpourri wherein.Preferred earlier organic dyestuff the mixing with the ratio of 0.01-0.1g/ (ml absolute ethyl alcohol) with absolute ethyl alcohol, for example can be with the 1g dyestuff: the ratio mixing of 10ml absolute ethyl alcohol, water be towards rare 100 times then.
According to another kind of preferred embodiment, in step (c), carry out painted processing with humidity chromogenic indicator of the present invention before, among or afterwards, preferred before or after, water cleans silica gel particle, and then carries out drying.
By embodiment the present invention is described in detail below, but should be pointed out that these embodiment are used to explain the present invention, rather than limitation of the present invention.
Embodiment
The Kiselgel A that adopts in the following examples: granularity 0.5-2mm, 2-5mm, more than the 5mm, average pore size 20-30 , specific surface area 600m
2More than/the g, more than the bulk density 600g/l.Company limited produces and sells by the U.S. high chemical industry in Qingdao.
Embodiment 1
The granularity that 5kg moisture absorption is good is the ethanol/water (ethanol: mixed solution water=1: 90) that the Kiselgel A of 2-5.6mm is put into the Acid Light Yellow G of 4000ml 0.1g/l, soaked 30 minutes, pull out and put into again in the humidity chromogenic indicator, humidity chromogenic indicator is the ferric chloride aqueous solutions of 10wt% by 4000ml concentration, 100ml concentration is that the ethanolic solution of the bromine phenols dyestuff of 0.1wt% mixes, soak after 2.5 hours, under 110 ℃, dry to moisture content below 4wt%, analyze data and see Table 1.
Embodiment 2
The granularity that 5kg moisture absorption is good is the ethanol/water (ethanol: mixed solution water=1: 90) that the Kiselgel A of 2-5mm is put into the acid brilliant yellow 2g of 0.5g/l, the dye liquor amount is 4000ml, soaked 1 hour, pull out and put into again that (humidity chromogenic indicator is by the ethanolic solution of the methyl red of 100ml0.1wt% in the humidity chromogenic indicator that has prepared, the ethanolic solution and the ferrous sulfate aqueous solution of the bromine phenols dyestuff of 100ml 0.1wt% are formulated, the cumulative volume of humidity chromogenic indicator is 4000ml, the concentration of ferrous sulphate is 25%), soak after 2 hours, oven dry, 110 ℃ of bake out temperatures to moisture content below 4%, analyze data and see Table 2.
Embodiment 3
The granularity that 2.5kg moisture absorption is good is the ethanol/water (ethanol: mixed solution water=1: 90) that the Kiselgel A of 0.5-2mm is put into the acid scarlet of 1g/l, the dye liquor amount is 3000ml, soak after 1 hour, pull out and put into the 3000ml humidity chromogenic indicator again (humidity chromogenic indicator bromine phenols dyestuff accounts for 0.01wt%; Iron sulfate (III) ammonium accounts for 30wt%), to soak and pull oven dry moisture content after 2 hours out to 4wt%, the analytical applications data see the following form 3.
Embodiment 4
The granularity that 1kg moisture absorption is good is that the Kiselgel A more than the 5mm is put into 800ml, the ethanol/water of 0.6wt% yellow (Acid Light Yellow G) (ethanol: water=1: 90) in the mixed solution, soak after 1 hour, pull out again and put into that (it consists of bromine phenols dyestuff and thymol blue respectively accounts for 0.1wt% in the 800ml humidity chromogenic indicator, iron sulfate (III) ammonium accounts for 15wt%, potassium permanganate accounts for 2wt% and copper sulphate accounts for 0.5wt%, ethanol accounts for 11.25wt%, with the consumption of water be 720ml), soaked 2 hours, and under 110 ℃, dried then to moisture content (the analysis data see Table 4) below 4wt%.
Embodiment 5
The granularity that 3kg moisture absorption is good is that the Kiselgel A of 2-5.6mm is put into 2500ml, the ethanol/water of 0.5% acid brilliant yellow 2g (ethanol: water=1: 90) soak after 1 hour in the mixed solution, pull out again and put into that (wherein bromine phenols dyestuff accounts for 0.05wt% in the 2500ml humidity chromogenic indicator, iron sulfate (III) ammonium accounts for 20wt%), soaked 2 hours, pull out then dry to moisture content less than 4wt% (applied analysis data such as following table 5).
Table 1
| Adsorbance (%) | The colour developing situation | |||||
| 10 minutes | 20 minutes | 30 minutes | 60 minutes | After 2 hours | ||
| RH＝20％ | 8.93 | Constant | Constant | Slightly shoal a little | The ruddiness yellow | The ruddiness yellow |
| RH＝50％ | 24.73 | Slightly shoal a little | A gold-tinted is arranged | Band ruddiness yellow | Yellow | Yellow |
| RH＝80％ | 39.06 | The beginning flavescence | Yellow | Deep yellow | Golden yellow | Golden yellow |
| Outward appearance | Red | |||||
| Moisture content (%) | 1.5 | |||||
Table 2
| Adsorbance | The colour developing situation | |||||
| 10 minutes | 20 minutes | 30 minutes | 60 minutes | After 2 hours | ||
| RH＝20％ | 8.56 | Constant | Constant | Slightly shoal a little | The ruddiness yellow | The ruddiness yellow |
| RH＝50％ | 22.67 | Slightly shoal a little | A gold-tinted is arranged | Band ruddiness yellow | Yellow | Yellow |
| RH＝80％ | 39.88 | The beginning flavescence | Yellow | Deep yellow | Golden yellow | Golden yellow |
| Outward appearance | Red | |||||
| Moisture content (%) | 1.8 | |||||
Table 3
| Adsorbance | The colour developing situation | |||||
| 10 minutes | 20 minutes | 30 minutes | 60 minutes | After 2 hours | ||
| RH＝20％ | 9.42 | Constant | Constant | Slightly shoal a little | The ruddiness yellow | The ruddiness yellow |
| RH＝50％ | 25.18 | Slightly shoal a little | A gold-tinted is arranged | Band ruddiness yellow | Yellow | Yellow |
| RH＝80％ | 38.04 | The beginning flavescence | Yellow | Deep yellow | Golden yellow | Golden yellow |
| Outward appearance | Red | |||||
| Moisture content (%) | 1.5 | |||||
Table 4
| Adsorbance | The colour developing situation | |||||
| 10 minutes | 20 minutes | 30 minutes | 60 minutes | After 2 hours | ||
| RH＝20％ | 9.58 | Constant | Constant | Slightly shoal a little | The ruddiness yellow | The ruddiness yellow |
| RH＝50％ | 26.13 | Slightly shoal a little | A gold-tinted is arranged | Band ruddiness yellow | Yellow | Yellow |
| RH＝80％ | 39.04 | The beginning flavescence | Yellow | Deep yellow | Golden yellow | Golden yellow |
| Outward appearance | Red | |||||
| Moisture content (%) | 1.7 | |||||
Table 5
| Adsorbance (%) | The colour developing situation | |||||
| 10 minutes | 20 minutes | 30 minutes | 60 minutes | After 2 hours | ||
| RH＝20％ | 9.08 | Constant | Constant | Slightly shoal a little | The ruddiness yellow | The ruddiness yellow |
| RH＝50％ | 25.68 | Slightly shoal a little | A gold-tinted is arranged | Band ruddiness yellow | Yellow | Yellow |
| RH＝80％ | 38.08 | The beginning flavescence | Yellow | Deep yellow | Golden yellow | Golden yellow |
| Outward appearance | Red | |||||
| Moisture content (%) | 1.8 | |||||
Regeneration embodiment 1
The discolour silica gel 200g that obtains among the embodiment 3 is placed in the air, static 24 hours (silicon particle will be individual layer dew and put with abundant absorption moisture), and then put into baking oven, and dried 2 hours down at 110 ℃, cooling, test result is as shown in table 6.
Get the discolour silica gel 500g that obtains among the embodiment 3, repeat the test described in the last period every day, repeat after six days, test result is as shown in table 7.
Table 6
| Adsorbance | The colour developing situation | |||||
| 10 minutes | 20 minutes | 30 minutes | 60 minutes | After 2 hours | ||
| RH＝20％ | 9.38 | Constant | Constant | Slightly shoal a little | The ruddiness yellow | The ruddiness yellow |
| RH＝50％ | 25.04 | Slightly shoal a little | A flavescence is arranged | The ruddiness yellow | Yellow | Yellow |
| RH＝80％ | 38.21 | The beginning flavescence | Yellow | Deep yellow | Golden yellow | Golden yellow |
| Outward appearance | Red | |||||
| Moisture content (%) | 1.5 | |||||
Table 7
| Adsorbance (%) | The colour developing situation | |||||
| 10 minutes | 20 minutes | 30 minutes | 60 minutes | After 2 hours | ||
| RH＝20％ | 9.30 | Constant | Constant | Slightly shoal a little | The ruddiness yellow | The ruddiness yellow |
| RH＝50％ | 24.87 | Slightly shoal a little | A flavescence is arranged | The ruddiness yellow | Yellow | Yellow |
| RH＝80％ | 37.64 | The beginning flavescence | Yellow | Deep yellow | Golden yellow | Golden yellow |
| Outward appearance | Red | |||||
| Moisture content (%) | 1.9 | |||||
Industrial applicibility
Compare with the cobalt humidity chromogenic indicator that contains of prior art, humidity chromogenic indicator of the present invention has obvious advantage. As previously mentioned, because it does not contain cobalt, but adopt cheap common inorganic salts as raw material, therefore greatly reduce production cost, avoided simultaneously the toxicity of cobalt and radioactivity to the harm of human body and environment. When the cost when adopting humidity chromogenic indicator of the present invention to produce discolour silica gel only is equivalent to cobalt chloride 1/10. In addition, when producing discolour silica gel, adopt indicator of the present invention can greatly reduce scrap rubber amount (scrap rubber amount only be equivalent to use other indicator 1/3), thereby significantly improved productive rate.
In like manner, compare with the discolour silica gel of prior art, discolour silica gel low production cost of the present invention is nontoxic, "dead". In addition, preparation is simple, and product can repeatedly regenerate and reuse, and it is clear to develop the color, and variable color is sensitive, and appearance luster is even, beautiful, and on the data of embodiment indication, the product that uses the present invention to produce is better than containing the cobalt discolour silica gel.
Claims (6)
1. discolour silica gel humidity chromogenic indicator, it contains organic solvent, general assembly (TW) in final indicator, the inorganic salts of 10-40wt%, colourity indicator with 0.1wt%-5wt%, and do not contain cobalt, wherein said organic solvent is selected from absolute ethyl alcohol, 95% ethanol, ethylene glycol, glycerine, in isopropyl alcohol and the n-propanol one or more, wherein said inorganic salts are selected from ferric trichloride, ferrous sulphate, iron sulfate (III) ammonium, in potassium permanganate and the copper sulphate one or more, wherein said colourity indicator is selected from phenolphthalein, reindeer moss, bromine phenols dyestuff, thymol blue, methyl red, orange N and two or more potpourri wherein.
2. humidity chromogenic indicator as claimed in claim 1, wherein said inorganic salts are selected from ferric trichloride, one or more in iron sulfate (III) ammonium and the potassium permanganate.
3. humidity chromogenic indicator as claimed in claim 1, the content of wherein said inorganic salts are 10-30wt%.
4. discolour silica gel, it contains the inorganic salts of 0.1-4.5wt%, the colourity indicator of 0.01-0.03wt%, the organic dyestuff of 0.001-0.01wt% and as the granular colloidal silica with nano micropore structure capable of surplus, wherein said inorganic salts are selected from ferric trichloride, ferrous sulphate, iron sulfate (III) ammonium, in potassium permanganate and the copper sulphate one or more, do not contain cobalt salt, wherein said colourity indicator is selected from phenolphthalein, reindeer moss, bromine phenols dyestuff, thymol blue, methyl red, orange N and two or more potpourri wherein, wherein said organic dyestuff is selected from polar yellow GN, Acid Light Yellow G, acid brilliant yellow 2g, acid scarlet, alkaline pink, gentian violet and two or more potpourri wherein
Described discolour silica gel is prepared by a method comprising the following steps:
(a) moisture absorption has nanometer level microporous Kiselgel A, moisture absorption to be put in do not burst in the tap water till;
(b) will contaminate in advance in the immersion of the Kiselgel A after the moisture absorption organic dyestuff solution;
(c) will in the silica gel of pre-dip-dye immerses among the claim 1-3 each humidity chromogenic indicator solution, contaminate, take out dry then.
5. discolour silica gel as claimed in claim 4, the described pre-dip-dye time is 1-1.5 hour.
6. discolour silica gel as claimed in claim 4, wherein said inorganic salts are selected from ferric trichloride, one or more in iron sulfate (III) ammonium and the potassium permanganate.
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|---|---|---|---|
| CN 02127021 CN1238719C (en) | 2002-07-25 | 2002-07-25 | Humidity chromogenic indicator and chromatropic silica gel prepared therwith and its preparing method |
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| CN 02127021 CN1238719C (en) | 2002-07-25 | 2002-07-25 | Humidity chromogenic indicator and chromatropic silica gel prepared therwith and its preparing method |
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| CN1238719C true CN1238719C (en) | 2006-01-25 |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101875496B (en) * | 2009-04-30 | 2013-03-27 | 北京金伟晖工程技术有限公司 | Recovering method of silica gel used for petroleum product fluorescent group composition analysis |
| CN103091321A (en) * | 2012-12-25 | 2013-05-08 | 山东辛化硅胶有限公司 | Cobaltless blue color-changing indicator and production method thereof |
| CN104406745B (en) * | 2014-11-05 | 2017-04-12 | 北京卫星环境工程研究所 | Portable flexible moist containing work medium leakage detection sticker and leakage detection method thereof |
| CN105784704A (en) * | 2016-03-11 | 2016-07-20 | 国家电网公司 | Portable color display device for flue gas humidity |
| CN106004158A (en) * | 2016-06-30 | 2016-10-12 | 李宝 | Dampproof portfolio |
| CN106198533B (en) * | 2016-08-17 | 2019-01-11 | 沈阳农业大学 | It is a kind of for detecting the humidity indicator and preparation method thereof of crop leaf humidity |
| CN109173627B (en) * | 2018-10-25 | 2021-04-09 | 青岛美高集团有限公司 | Preparation method of allochroic silica gel drying agent and allochroic silica gel prepared by same |
| CN112285271A (en) * | 2020-10-22 | 2021-01-29 | 东来涂料技术（上海）股份有限公司 | Method for judging moisture content of organic solvent |
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