CN1128361C - Multi-colour allochromatic indicator and its producing method - Google Patents
Multi-colour allochromatic indicator and its producing method Download PDFInfo
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Abstract
The present invention relates to a color discoloring indicator and a production method thereof. Tangible granule adsorbing agents, such as silicon dioxide, etc., are processed by dyeing liquid, such as bromcresol green, bromchlorphenol blue, methyl red, crystal violet, neutral red, methyl orange, malachite green, green phenol red and bromothymol blue, to prepare nine indicator finished products of which the colors are reversely changed following different water containing degrees, such as yellow adhesives I, II, III, IV, V, red adhesives I, II, III and lac I. The indicator products can be used for drying or indicating humidity, indicating acid and base gas compositions in the environment and reducing environmental pollution. The color discoloring indicator can be used for the technical processing of dehumidification, moisture display, purification, etc. in the industrial fields of war industry, textiles, chemical industry, petroleum, furniture, etc.
Description
The present invention relates to the improvement of silica gel product, specifically is a kind of color discoloring indicator and production method thereof.It belongs to technical field of inorganic chemical industry.
Common inorganic adsorbent has: silica gel, Alusil, molecular sieve, aluminium oxide etc.These adsorbents can be used for dry relevant environment.A kind of blue-gel indicator is arranged, and it can show moisture absorption degree or degree of drying intuitively by change color.But to use cobalt chloride (CoCL in the manufacture method of this glue
2), this compound has been listed in two class carcinogenic substances through the research of external relevant department.Therefore use for a long time or make blue glue and can harm be arranged to operating personnel's health, some countries have determined progressively to stop using blue glue at present.Also have by phenolphthalein red cresols, the adsorbent that thymol blue is contaminated, the performance that can Show Color changes.The dyeing indicator that above-mentioned colour developing adsorbent is selected, its molecular weight is all less, so the painted absorption ratio of these indicator is easier to.Yet for the big dyeing indicator of molecular weight, as: the molecular weight of bromcresol green is 698.07; The molecular weight of bromjophenol blue is 670.02; The molecular weight of bromine thymol blue is 624; These big relatively dyeing indicator are to be difficult to painted absorption to the adsorbent of general dry state.Because the molecule of dyeing indicator is generally all quite big, big have 698.07 of a bromcresol green, and little also has: 269.3 of methyl red, 288.78 of dimethyl diaminophenazine chloride, 327.34 of methyl orange.So just make dried glue and wet glue to the adsorption coloring of above-mentioned dyeing liquor very crucial influence be arranged, promptly dried glue only can the less dyeing liquor of absorbing molecules amount.
The objective of the invention is to provide a kind of color discoloring indicator.The appearance luster of this indicator can the reversible variation along with the difference of moisture degree.It is wide that the color range of choice of its colour developing is wanted, and is not limited only to the redden blue glue of look of blueness.Enlarge the scope and the application choice scope of dyeing liquor indication color, more dyeing liquor is used in the manufacturing process of adsorption indicator.Improve process conditions, make the dyed PROCESS FOR TREATMENT of applied adsorbent material after, color obviously and is uniformly arranged.This indicator also will keep the original performance of former adsorbent constant, and increases the performance of the moisture degree of colour developing indication.
Task of the present invention is realized by following technical scheme, has developed a kind of color discoloring indicator, and it is by silica gel, Alusil, molecular sieve, aluminium oxide, magnesium oxide, the tangible granule adsorbent of titanium dioxide, dyed liquid are handled and are made the color discoloring indicator with following physical and chemical indexes:
Adsorbance, RH is at 20% o'clock, and 〉=9.0%; RH was at 50% o'clock; 〉=22.0%; The granularity qualification rate, 〉=90.0%; Heating loss ,≤5.0%; In reversible colour developing changed, the reversible color scope of all this indicator indications was:
The production method of this color discoloring indicator is with silica gel, Alusil, molecular sieve, aluminium oxide, magnesium oxide, in the tangible granule adsorbent of titanium dioxide one or more, the processing of dyeing, select aforementioned this adsorbent hygrometric state or/and the dry state material immerse in proportion and contain in the aqueous solution of dyeing liquor, contaminated at normal temperatures 2-48 hour, then leach and wash to wash water be colourless till, pull the material of dip-dye at last out, drying is handled, bake out temperature: 80-140 ℃, make color discoloring indicator.
Described dyeing liquor, it comprises: bromcresol green, bromjophenol blue, methyl red, methyl violet, green phenol red, dimethyl diaminophenazine chloride, methyl orange, peacock green, bromine thymol blue; Wherein by bromcresol green make yellow glue I indicator; By bromjophenol blue make yellow glue II indicator; By methyl red make yellow glue III indicator; By methyl violet make yellow glue IV indicator; By bromjophenol blue and cresols green make yellow glue V indicator; By dimethyl diaminophenazine chloride make red glue I indicator; By methyl orange make red glue II indicator; By peacock green make red glue III indicator; By the bromine thymol blue make lac I indicator.
The aqueous solution of described dyeing liquor, its bulking value specific concentration is: 0.001～5.00%; To control the pH value of staining solution in the dyeing course 0～10.0.
The adjusting of described staining solution pH value can be selected phosphoric acid for use, or carbonate, or hydrochloric acid, or sulfuric acid, or among citric acid or the tartrate one or more.
The volume ratio of described hygrometric state or dry state material and dyeing liquor solution is (2.5-2.0): 1.
The invention has the advantages that: because the present invention has abandoned carcinogen and has been used to make indicator, this just provides guarantee for health environment-friendly.Owing to enlarge the range of choice of dyeing liquor, selected nine kinds of dyeing (indication) liquid, to the processing of dyeing of adsorbent material, made through the optimized process conditions processing: yellow glue indicator, red glue indicator, the color discoloring indicator of nine kinds of colour developings of lac indicator is used to indicate humid environment degree and degree of drying; Be used for the protection against the tide of instrument and meter equipment, anti-corrosion; The dehydration that is used for chemical products is refining, as the water treatment that removes of petroleum chemicals; The damp-prrof packing that is used for food industry, fresh-keeping guaranteeing the quality; Be widely used in military project, weaving, fields such as furniture.Owing to enlarged the adsorbent raw material sources, the glue that will wet directly applies in the dyeing, obtains the indicator of the various this patent of the higher pattern of quality quality, has enlarged the adsorbent range of application.Owing in dyeing, select different staining solution pH values, comprised the controlled variable in the acid and alkaline vast scope.Finished product color discoloring indicator of the present invention absorbs moisture between RH:10-50%, can have obvious color to change.Thereby indicate dry condition and moisture absorption degree intuitively.Simultaneously, this indicator that has changed color because of absorption moisture can heat the color of recovering original finished product color discoloring indicator between 80-180 ℃, therefore can continue to use.This indicator of the present invention can be used for absorbing moisture in the neutral gas, as: rock gas, N
2, O
2, H
2, CO
2, gaseous hydrocarbon, synthetic gas, pressurized air is carried gas etc.This indicator also can be used for indicating the soda acid composition in the neutral gas.
Embodiments of the invention will further specify superiority of the present invention.Protection scope of the present invention is not limited only among the present embodiment.
Color discoloring indicator of the present invention, by wet silica gel, dyed liquid is handled, and obtains the product of following technical feature indication: see Table 1, the performance index of product technologies measured data table 1 of color discoloring indicator:
The granule adsorbent that the present invention selects for use, its granularity is at 0.5-8.0mm.This adsorbent is to adopt conventional known method preparation.It has dry state gel (dried glue) and hydrogel (wet glue does not just have the semi-manufacture silica gel of drying).No matter dried glue is contaminated solution concentration and how to be changed for macromolecular dyeing liquor, in feasible pH value scope, and the adsorption indicator of gained, colourless substantially.See Table 2, table 3, experimental result: table 2, dried glue dyeing experimental result table:
| The adsorbent state | Indicator | The concentration % of staining solution | The control pH value | Finished product dry state indicator color |
| Dry state | Bromcresol green | 0.01％ | 4.1 | Substantially colourless |
| Dry state | Bromcresol green | 0.02％ | 4.5 | Substantially colourless |
| Dry state | Bromcresol green | 0.1％ | 4.8 | Substantially colourless |
| Dry state | Bromcresol green | 0.1％ | 5.3 | Substantially colourless |
| Dry state | Bromjophenol blue | 0.001％ | 3.7 | Substantially colourless |
| Dry state | Bromjophenol blue | 0.002％ | 4.7 | Substantially colourless |
| Dry state | Bromjophenol blue | 0.01％ | 5.2 | Substantially colourless |
| Dry state | Bromjophenol blue | 0.1％ | 6.0 | Substantially colourless |
Table 3: wet glue dyeing experimental result table.
| The adsorbent state | Indicator | The concentration % of staining solution | The control pH value | Finished product dry state indicator color |
| Hygrometric state | Bromcresol green | 0.001％ | 3.9 | Light yellow |
| Hygrometric state | Bromcresol green | 0.002％ | 4.3 | Light yellow |
| Hygrometric state | Bromcresol green | 0.01％ | 4.8 | Light yellow |
| Hygrometric state | Bromcresol green | 0.005％ | 5.3 | Light green color |
| Hygrometric state | Bromjophenol blue | 0.005％ | 4.8 | Light yellow |
| Hygrometric state | Bromjophenol blue | 0.01％ | 5.5 | Light brown |
| Hygrometric state | Bromjophenol blue | 0.01％ | 6.4 | Lilac |
Can find out from table 2,3: wet deadlocked look performance is good.This be since aperture, pore volume and the specific surface area of wet glue all greater than the relevant parameter of dried glue, gap 7-10 is doubly on its data.
Generally want elder generation through the steam moisture absorption owing to contaminate indicator, can cause adsorbance to descend like this, therefore, can reduce cost, higher adsorbance is arranged simultaneously with the color discoloring indicator of wet glue dip-dye preparation with dried glue.See Table 4, table 4: dry method and wet method are contaminated the comparison of gained indicator product adsorbance
| Indicator | Former adsorbent state | The adsorbance of finished product indicator | |
| RH20％ | RH50％ | ||
| The bromine thymol blue | Dried glue | 10.1 | 25.7 |
| The bromine thymol blue | Dried glue | 9.5 | 24.1 |
| The bromine thymol blue | Dried glue | 9.5 | 23.9 |
| The bromine thymol blue | Wet glue | 9.9 | 27.6 |
| The bromine thymol blue | Wet glue | 10.3 | 28.3 |
| The bromine Thymol is a little | Wet glue | 10.5 | 27.9 |
(1) embodiment of yellow glue II indicator production: with the bromjophenol blue is that the indication dye dip is dyed wet glue, under variable concentrations, contaminate wet glue, and use different soda acid control to contaminate the pH value of solution between 3.0-7.5, contaminate after 24-48 hour, it is colourless being washed to wash water, in 120 ℃ ± 5 ℃ oven dry down of uniform temp, the results are shown in Table 5: table 5: the embodiment that yellow glue II indicator is produced again:
| Instance number | Indicator dye | Concentration W/V% | Used acid or alkali | The control pH value | Oven dry back color | Suction back color |
| 1 | Bromjophenol blue | 0.004 | Sulfuric acid | 3.5 | Light yellow | Light yellow |
| 2 | Bromjophenol blue | 0.004 | Sulfuric acid | 3.8 | Light yellow | Light brown |
| 3 | Bromjophenol blue | 0.004 | Phosphoric acid | 4.3 | Light yellow | Brown |
| 4 | Bromjophenol blue | 0.003 | Phosphoric acid | 4.7 | Light yellow | Lilac |
| 5 | Bromjophenol blue | 0.003 | Tartrate | 5.5 | Light brown | Lilac |
| 6 | Bromjophenol blue | 0.01 | Tartrate | 6.4 | Lilac | Lilac |
(2) production example of yellow glue I indicator:
Indicate dyeing liquor to contaminate wet glue with bromcresol green, and control dip-dye solution pH value is operated result such as table 6 at 4.0-5.0 to shine said method:
Table 6: the production example of yellow glue I indicator:
| Instance number | Indicator dye | Concentration (W/V%) | Used acid or alkali | The control pH value | Oven dry back color | Suction back color |
| 7 | Bromcresol green | 0.005 | Sulfuric acid | 3.5 | Light yellow | Light yellow |
| 8 | Bromcresol green | 0.005 | Phosphoric acid | 4.1 | Light yellow | Light green color |
| 9 | Bromcresol green | 0.01 | Phosphoric acid | 4.8 | Light yellow | Bottle green |
| 10 | Bromcresol green | 0.01 | Phosphoric acid | 5.2 | Light green color | Bottle green |
| 11 | Bromcresol green | 0.012 | Citric acid | 6.3 | Light blue | Light blue |
(3) embodiment of lac I production:
Contaminate in Alusil with the bromine thymol blue, and control dip-dye solution pH value is operated gained result such as table 7 at 5.0-9.0 with method same as described above:
Table 7: the production example of lac I indicator:
| Instance number | Indicator dye | Concentration (W/V%) | Used acid or alkali | The control pH value | Oven dry back color | Suction back color |
| 12 | The bromine thymol blue | 0.02 | Phosphoric acid | 5.1 | Lilac | Shallow salmon pink |
| 13 | The bromine thymol blue | 0.02 | Phosphoric acid | 5.9 | Lilac | Shallow salmon pink |
| 14 | The bromine thymol blue | 0.05 | Phosphoric acid | 6.8 | Lilac | Shallow salmon pink |
| 15 | The bromine thymol blue | 0.1 | Sodium carbonate | 7.5 | Lilac | Shallow salmon pink |
(4) production example of yellow glue III indicator:
Contaminate silica gel with methyl red, control is contaminated the pH value of solution between 8.0-9.0, according to the said method operation, and result such as table 8:
Table 8: the production example of yellow glue III indicator:
| Instance number | Indicator dye | Concentration (W/V%) | Used acid or alkali | The control pH value | Oven dry back color | Suction back color |
| 16 | Methyl red | 0.01 | Hartshorn salt | 7.1 | Light yellow | Light yellow |
| 17 | Methyl red | 0.01 | Hartshorn salt | 7.7 | Light yellow | Light yellow |
| 18 | Methyl red | 0.02 | Sodium carbonate | 8.2 | Light yellow | Shallow salmon pink |
| 19 | Methyl red | 0.03 | Sodium carbonate | 8.5 | The light orange look | Shallow salmon pink |
| 20 | Methyl red | 0.05 | Sodium carbonate | 8.9 | Orange colour | Salmon pink |
(5) production example of red glue I indicator:
With the dimethyl diaminophenazine chloride is dyestuff, and control is contaminated the pH value of solution between 7.0-8.5.Contaminate with method of the present invention.Gained result such as table 9:
Table 9: the production example of red glue I indicator:
| Instance number | Indicator dye | Concentration (W/V%) | Used acid or alkali | The control pH value | Oven dry back color | Suction back color |
| 21 | Dimethyl diaminophenazine chloride | 0.025 | Sulfuric acid | 5.7 | Peony | Peony |
| 22 | Dimethyl diaminophenazine chloride | 0.025 | Phosphoric acid | 6.4 | Peony | Peony |
| 23 | Dimethyl diaminophenazine chloride | 0.05 | Sodium carbonate | 7.6 | Peony | Light red |
| 24 | Dimethyl diaminophenazine chloride | 0.05 | Sodium carbonate | 8.1 | Peony | Light red |
| 25 | Dimethyl diaminophenazine chloride | 0.1 | Sodium carbonate | 8.8 | Peony | Peony |
(6) production example of red glue II:
With methyl orange is indicator, and control is contaminated the pH value of solution between 4.0-7.0, operates result such as table 10 by method of the present invention:
Table 10: the production example of red glue II indicator:
| Instance number | Indicator dye | Concentration (W/V%) | Used acid or alkali | The control pH value | Oven dry back color | Suction back color |
| 26 | Methyl orange | 0.025 | Sulfuric acid | 3.5 | Peony | Peony |
| 27 | Methyl orange | 0.05 | Phosphoric acid | 5.7 | Peony | Orange-yellow |
| 28 | Methyl orange | 0.01 | Sodium carbonate | 7.9 | Peony | Peony |
(7) embodiment of yellow glue IV indicator production:
With methyl violet is dyestuff, contaminates silica gel in different concentration, and with different acid control pH value 0-1.5, contaminates after 24 hours, and it is colourless being washed to wash water, dry under 100 ℃ ± 5 ℃, the results are shown in Table 11:
Table 11: the production example of yellow glue IV indicator:
| Instance number | Dyestuff | Concentration (W/V%) | Used acid | Control PH | Dry back color | Color after the moisture absorption |
| 29 | Methyl violet | 0.01 | Sulfuric acid | 0.6 | Light yellow | Light green color |
| 30 | Methyl violet | 0.02 | Sulfuric acid | 0.8 | Light yellow | Light green color |
| 31 | Methyl violet | 0.01 | Sulfuric acid | 0.2 | Light yellow | Light green color |
| 32 | Methyl violet | 0.01 | Sulfuric acid | 0.3 | Light yellow | Pale bluish green |
| 33 | Methyl violet | 0.01 | Sulfuric acid | 0.4 | Light yellow | Pale bluish green |
| 34 | Methyl violet | 0.02 | Sulfuric acid | 0.5 | Light yellow | Pale bluish green |
(8) production example of yellow glue V indicator:
With bromjophenol blue and the green phenol red dyestuff of doing jointly, under the variable concentrations pH value, contaminated 24 hours, it is colourless to be washed to wash water, then 100 ℃ ± 5 ℃ oven dry down, the results are shown in Table 12:
Table 12: the production example of yellow glue V indicator:
| Instance number | Dyestuff | Concentration (W/V%) | Acid or alkali | The control pH value | Oven dry back color | Color after the moisture absorption |
| 35 | Bromjophenol blue is green phenol red | 0.02 0.02 | Sodium carbonate | 7 | Light yellow | Light brown |
| 36 | Bromjophenol blue is green phenol red | 0.03 0.03 | Sodium carbonate | 8 | Light yellow | Light brown |
(9) production example of red glue III indicator:
Make dyestuff with peacock green, contaminate to carry out 24hr under variable concentrations and the pH value, and post-flush is colourless to wash water, oven dry.The result is as follows, sees Table 13:
Table 13: the production example of red glue III indicator:
| Instance number | Dyestuff | Concentration (W/V%) | Used acid | Control PH | Oven dry back color | Color after the moisture absorption |
| 37 | Peacock green | 0.03 | Sulfuric acid | 0.2 | Shallow salmon pink | Shallow blackish green |
| 38 | Peacock green | 0.04 | Phosphoric acid | 0.8 | Light red | Shallow blackish green |
| 39 | Peacock green | 0.06 | Hydrochloric acid | 1.2 | Light red | Shallow blackish green |
| 40 | Peacock green | 0.03 | Sulfuric acid | 0.4 | Shallow salmon pink | Shallow blackish green |
| 41 | Peacock green | 0.04 | Phosphoric acid | 0.4 | Shallow salmon pink | Shallow blackish green |
| 42 | Peacock green | 0.06 | Hydrochloric acid | 0.5 | Shallow salmon pink | Shallow blackish green |
| 43 | Peacock green | 0.06 | Hydrochloric acid | 0.6 | Shallow salmon pink | Shallow blackish green |
Claims (5)
1, a kind of color discoloring indicator, it is by silica gel, Alusil, molecular sieve, aluminium oxide, magnesium oxide, the tangible granule adsorbent of titanium dioxide, dyed liquid are handled and are made the color discoloring indicator with following physical and chemical indexes: adsorbance, RH is at 20% o'clock, and 〉=9.0%; RH was at 50% o'clock; 〉=22.0%; The granularity qualification rate, 〉=90.0%; Heating loss ,≤5.0%; It is characterized in that: dyed liquid is handled the color discoloring indicator that makes and is: the yellow glue I indicator that is made by bromcresol green; The yellow glue II indicator that makes by bromjophenol blue; The yellow glue III indicator that makes by methyl red; The yellow glue IV indicator that makes by methyl violet; By bromjophenol blue and the green phenol red yellow glue V indicator that makes; The red glue I indicator that makes by dimethyl diaminophenazine chloride; The red glue II indicator that makes by methyl orange; The red glue III indicator that makes by peacock green; The lac I indicator that makes by the bromine thymol blue; In reversible colour developing changed, the reversible color scope of all this indicator indications was:
2, the production method of color discoloring indicator according to claim 1, be with silica gel, Alusil, molecular sieve, aluminium oxide, magnesium oxide, one or more in the tangible granule adsorbent of titanium dioxide, the processing of dyeing, it is characterized in that: the hygrometric state of selecting aforementioned this adsorbent is or/and the dry state material, immerse in proportion and contain in the aqueous solution of dyeing liquor, contaminated at normal temperatures 2-48 hour, then leach and wash to wash water be colourless till, pull the material of dip-dye at last out, drying is handled, and bake out temperature: 80-140 ℃, makes color discoloring indicator.
3, the production method of color discoloring indicator according to claim 2 is characterized in that: the aqueous solution of described dyeing liquor, and its bulking value specific concentration is: 0.001-5.00%; To control the pH value of staining solution in the dyeing course 0～10.0.
4, the production method of color discoloring indicator according to claim 3 is characterized in that: the adjusting of described staining solution pH value, can select phosphoric acid for use, or carbonate, or hydrochloric acid, or sulfuric acid, or among citric acid or the tartrate one or more.
5, according to the production method of claim 2 or 3 described color discoloring indicators, it is characterized in that: described hygrometric state is or/and the volume ratio of dry state material and dyeing liquor solution is (2.5-2.0): 1.
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|---|---|---|---|
| CN 00111177 CN1128361C (en) | 2000-03-24 | 2000-07-07 | Multi-colour allochromatic indicator and its producing method |
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|---|---|---|---|
| CN00110956.1 | 2000-03-24 | ||
| CN 00110956 CN1269507A (en) | 2000-03-24 | 2000-03-24 | Color discoloring indicator and its production process |
| CN 00111177 CN1128361C (en) | 2000-03-24 | 2000-07-07 | Multi-colour allochromatic indicator and its producing method |
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| CN1128361C true CN1128361C (en) | 2003-11-19 |
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| AU2003219800A1 (en) * | 2002-02-19 | 2003-09-09 | The Procter And Gamble Company | Wetness indicator having improved colorant retention and durability |
| US20110104023A1 (en) * | 2008-06-25 | 2011-05-05 | Kyodo Printing Co., Ltd. | Humidity indicator and method for producing the same |
| CN101710056B (en) * | 2009-10-29 | 2012-07-04 | 中国农业科学院植物保护研究所 | Test card for testing wettability of spray liquor and preparation method thereof |
| 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 |
| CN107110771A (en) * | 2014-11-07 | 2017-08-29 | 水透镜公司 | Composition, apparatus and method for the basicity that determines analyte solution |
| CN105865652B (en) * | 2016-03-30 | 2018-11-23 | 深圳九星印刷包装集团有限公司 | Instruction device and preparation method thereof |
| CN109052414A (en) * | 2018-08-17 | 2018-12-21 | 山东辛化硅胶有限公司 | A kind of multistage humidity instruction Silica hydrogel and preparation method thereof |
| CN108801367A (en) * | 2018-09-07 | 2018-11-13 | 浙江健拓医疗仪器科技有限公司 | A kind of environmental detection set and its manufacturing method suitable for poct class diagnostic reagents |
| CN111617734B (en) * | 2020-05-27 | 2022-07-05 | 青岛华世洁环保科技有限公司 | Color-changeable amine deodorization material |
| CN111662702A (en) * | 2020-06-17 | 2020-09-15 | 厦门安踏体育用品有限公司 | Inductive color-changing material and application thereof in garment fabric |
| CN113402734B (en) * | 2021-06-17 | 2023-04-18 | 东北农业大学 | Preparation method and application of hydrogel for indicating freshness of chilled meat |
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