CN109439018A - The method in small particle color lake is prepared in a kind of continuous flow micro passage reaction - Google Patents
The method in small particle color lake is prepared in a kind of continuous flow micro passage reaction Download PDFInfo
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- CN109439018A CN109439018A CN201811592470.6A CN201811592470A CN109439018A CN 109439018 A CN109439018 A CN 109439018A CN 201811592470 A CN201811592470 A CN 201811592470A CN 109439018 A CN109439018 A CN 109439018A
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- color lake
- reaction
- sodium bicarbonate
- micro passage
- solution
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B63/00—Lakes
- C09B63/005—Metal lakes of dyes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
Abstract
The invention discloses a kind of methods that small particle color lake is prepared in continuous flow micro passage reaction, include the following steps: step 1: preparing aluminium chloride and sodium bicarbonate solution；Step 2: liquor alumini chloridi and sodium bicarbonate solution are passed through in micro passage reaction by metering pump and carry out the preparation reaction of aluminium hydroxide carrier, coutroi velocity, aluminium chloride and sodium bicarbonate molar ratio, reaction temperature, residence time of the reaction solution in micro passage reaction, aluminium hydroxide suspension is obtained after reflection, and it is spare to be obtained into active aluminium hydroxide for aluminium hydroxide suspension filtration washing；Step 3: color lake preparation step；Step 4: less than 1.5 μm color lake products of partial size are obtained after chloride ion processing is dispelled in color lake.The present invention is by the reinforcing mass transfer of microchannel apparatus, and many experiments adjust and strengthen mixed effect, to be prepared for the active aluminium hydroxide matrix of small particle, and by load pigment, available partial size is lower than 1 μm of color lake.
Description
Technical field
The invention belongs to color lake preparation fields, and in particular to small particle color lake is prepared in a kind of continuous flow micro passage reaction
Method.
Background technique
Color lake is that soluble dye forms precipitating under alkaline condition or is combined into metal hydroxides water-insoluble
Pigment, there is the advantages of water-insoluble, anti-pigment migration, high security and stability.The product quality in color lake is by partial size shadow
Sound is larger, if forming the aluminium hydroxide carrier compared with small particle, the pigment uniformity and coloring effect of load are more outstanding, simultaneously
Specific surface area increases, during chloride ion is washed in post-processing also advantageously.
Existing color lake production technology carries out in a kettle, obtains the hydrogen compared with small particle with slowly feeding intake by stirring
Aluminium oxide, existing technique can make the partial size in color lake reach 1-5 μm, but traditional tank reactor is limited due to itself, is existed
The slower unfavorable factor of heat and mass, leads to the defects of reaction time is too long, and back-mixing is larger, and reaction controlling is not sufficiently stable.
Summary of the invention
In order to overcome the drawbacks described above of the prior art, the purpose of the present invention is to provide a kind of continuous flow micro passage reactions
The method in middle preparation small particle color lake improves product quality and production stability to reduce diameter of carrier.
One of in order to achieve the object of the present invention, used technical solution is:
A kind of method that small particle color lake is prepared in continuous flow micro passage reaction, includes the following steps:
Step 1: aluminium chloride and sodium bicarbonate solution are prepared, wherein the concentration of the liquor alumini chloridi is 0.3-
0.8mol/L, the concentration of the sodium bicarbonate solution are 0.1-0.2mol/L；
Step 2: liquor alumini chloridi and sodium bicarbonate solution are passed through in micro passage reaction by metering pump and carry out hydrogen-oxygen
Change alumina supporter preparation reaction, coutroi velocity, keeps the aluminium chloride reacted and sodium bicarbonate molar ratio is 0.35-0.5, reaction
Temperature is 15-30 DEG C, and residence time of the reaction solution in micro passage reaction is 60-600s, obtains hydroxide after reflection
Aluminium hydroxide suspension filtration washing it is spare to be obtained active aluminium hydroxide by aluminium suspension；
Step 3: by the active aluminium hydroxide obtained in step 2, the mixing of synthetic food colors and aluminium chloride
Solution, for secondary hybrid reaction to form color lake, secondary mixed reaction temperature is 10-40 DEG C；
Step 4: the color lake that step 3 obtains is carried out to obtain color lake product after chloride ion processing is dispelled in washing, wherein institute
The partial size of color lake product is stated less than 1.5 μm.
In a preferred embodiment of the invention, the step one specifically: prepare aluminium chloride and sodium bicarbonate is molten
Liquid weighs sodium bicarbonate solid, is dissolved in distilled water, and being configured to concentration is 0.3-0.8mol/L solution, and it is solid to weigh aluminium chloride
Body is dissolved in distilled water, is configured to the solution that concentration is 0.1-0.2mol/L.
In a preferred embodiment of the invention, synthetic food colors described in the step 3 include it is carmine,
Lure red, sunset yellow, lemon yellow, brilliant blue, any one or more in erythrosine.
In a preferred embodiment of the invention, used in the mixed solution of the synthetic food colors and aluminium chloride
Pigment and raw material aluminium chloride molar ratio be 0.04-0.10.
In a preferred embodiment of the invention, the partial size of the color lake product is less than 1 μm.
Main innovation point of the invention is: present invention utilizes the reinforcing mass transfer of microchannel apparatus, having passed through a large amount of
Experiment is to adjust and strengthen mixed effect, so that the method for obtaining smaller particle product in the reaction is prepared for the activity of small particle
Aluminium hydroxide matrix, and by load pigment, available partial size is lower than 1 μm of color lake.
Specific embodiment
The present invention is described further with reference to embodiments:
Embodiment 1:
Microchannel apparatus is the FlowChemistrySystem of Vapourtec company, prepares liquor alumini chloridi and carbon respectively
Sour hydrogen sodium solution weighs 24.1g aluminium chlorohydrate and is configured to 500mL aqueous solution (0.2mol/L), weighs the preparation of 21g sodium bicarbonate
At 400mL aqueous solution (0.62mol/L), two kinds of materials are pumped into micro passage reaction by metering pump, the flow velocity of aluminium chloride is
The flow velocity of 2.78ml/min, sodium bicarbonate solution are 2.22ml/min, into the aluminium chloride and sodium bicarbonate molar ratio of reactor
It is 0.4, reaction temperature is 25 DEG C, and the residence time is 5 minutes, and obtained aluminium hydroxide suspension separately weighs rouge through filtration washing
The red solid 3.0g of rouge, pigment and chlorination al mole ratio are 0.05, prepare 2% cochineal solution, filter cake active aluminium hydroxide is carried
Body is added in carmine solution, filters after being heated with stirring to 40 DEG C of abundant reactions, filter cake is washed, famille rose is obtained
Color lake, measurement average grain diameter are 1.1 μm, pigment content 36.1%.
Embodiment 2:
Liquor alumini chloridi and sodium bicarbonate solution are prepared according to the condition and step of embodiment 1, two kinds of materials are passed through into meter
Amount is pumped into micro passage reaction, and the flow velocity of aluminium chloride is 4.63ml/min, and the flow velocity of sodium bicarbonate solution is 3.70ml/min,
Aluminium chloride and sodium bicarbonate molar ratio into reactor are 0.4, and reaction temperature is 25 DEG C, and the residence time is 3 minutes, are obtained
Aluminium hydroxide suspension separately weighs carmine solid 3.0g through filtration washing, and pigment and chlorination al mole ratio are 0.05, prepares
Filter cake active aluminium hydroxide carrier is added in carmine solution by 2% cochineal solution, is heated with stirring to 30 DEG C sufficiently instead
Should after filter, filter cake is washed, obtains carmine lake, measurement average grain diameter is 0.9 μm, pigment content 38.3%.
Embodiment 3:
Liquor alumini chloridi and sodium bicarbonate solution are prepared according to the condition and step of embodiment 1, two kinds of materials are passed through into meter
Amount is pumped into micro passage reaction, and the flow velocity of aluminium chloride is 4.63ml/min, and the flow velocity of sodium bicarbonate solution is 3.70ml/min,
Aluminium chloride and sodium bicarbonate molar ratio into reactor are 0.4, and reaction temperature is 30 DEG C, and the residence time is 3 minutes, are obtained
Aluminium hydroxide suspension separately weighs sunset yellow solid 5.4g through filtration washing, and pigment and chlorination al mole ratio are 0.12, prepares
Filter cake active aluminium hydroxide carrier is added in sunset yellow solution by 2% sunset yellow solution, is stirred under the conditions of 15 DEG C of temperature abundant
It is filtered after reaction, filter cake is washed, obtain sunset yellow lake, measurement average grain diameter is 0.9 μm, and pigment content is
37.5%.
Embodiment 4:
Liquor alumini chloridi and sodium bicarbonate solution are prepared, 24.1g aluminium chlorohydrate is weighed and is configured to 500mL aqueous solution
(0.2mol/L) weighs 23g sodium bicarbonate and is configured to 400mL aqueous solution (0.55mol/L), and two kinds of materials are pumped by metering pump
Enter micro passage reaction, the flow velocity of aluminium chloride is 2.78ml/min, and the flow velocity of sodium bicarbonate solution is 2.22ml/min, into anti-
It answers the aluminium chloride of device and sodium bicarbonate molar ratio is 0.35, reaction temperature is 20 DEG C, and the residence time is 5 minutes, obtained hydrogen-oxygen
Change aluminium suspension through filtration washing, separately weigh lemon yellow solid 3.1g, pigment and chlorination al mole ratio are 0.058, prepare 2% lemon
Filter cake active aluminium hydroxide carrier is added in the solution of lemon yellow by lemon Huang solution, after sufficiently reaction is stirred at 25 DEG C of room temperature
Filtering, filter cake is washed, and obtains lemon yellow color lake, and measurement average grain diameter is 0.9 μm, pigment content 36.8%.
Embodiment 5:
Liquor alumini chloridi and sodium bicarbonate solution are prepared, 24.1g aluminium chlorohydrate is weighed and is configured to 1000mL aqueous solution
(0.1mol/L) weighs 23g sodium bicarbonate and is configured to 800mL aqueous solution (0.55mol/L), and two kinds of materials are pumped by metering pump
Enter micro passage reaction, the flow velocity of aluminium chloride is 15.0ml/min, and the flow velocity of sodium bicarbonate solution is 10.0ml/min, into anti-
It answers the aluminium chloride of device and sodium bicarbonate molar ratio is 0.5, reaction temperature is 15 DEG C, and the residence time is 1 minute, obtained hydroxide
Aluminium suspension separately weighs the red solid 3.0g of temptation through filtration washing, and pigment and chlorination al mole ratio are 0.06, prepares 2% temptation
Filter cake active aluminium hydroxide carrier is added to and lures in red solution by red solution, is heated with stirring to mistake after 35 DEG C of abundant reactions
Filter, filter cake is washed, and obtains luring red shallow lake, measurement average grain diameter is 1.2 μm, pigment content 34.9%.
Embodiment 6:
Liquor alumini chloridi and sodium bicarbonate solution are prepared, 24.1g aluminium chlorohydrate is weighed and is configured to 500mL aqueous solution
(0.2mol/L) weighs 21g sodium bicarbonate and is configured to 800mL aqueous solution (0.62mol/L), and two kinds of materials are pumped by metering pump
Enter micro passage reaction, the flow velocity of aluminium chloride is 1.39ml/min, and the flow velocity of sodium bicarbonate solution is 1.11ml/min, into anti-
It answers the aluminium chloride of device and sodium bicarbonate molar ratio is 0.4, reaction temperature is 15 DEG C, and the residence time is 10 minutes, obtained hydrogen-oxygen
Change aluminium suspension through filtration washing, separately weigh brilliant blue solid 6.3g, pigment and chlorination al mole ratio are 0.08, prepare 2% brilliant blue
Filter cake active aluminium hydroxide carrier is added in the solution of brilliant blue by solution, is filtered after being heated with stirring to 40 DEG C of abundant reactions, will
Filter cake is washed, and brilliant blue color lake is obtained, and measurement average grain diameter is 1.4 μm, pigment content 38.7%.
Embodiment 7:
Liquor alumini chloridi and sodium bicarbonate solution are prepared, 24.1g aluminium chlorohydrate is weighed and is configured to 500mL aqueous solution
(0.2mol/L) weighs 21g sodium bicarbonate and is configured to 800mL aqueous solution (0.62mol/L), and two kinds of materials are pumped by metering pump
Enter micro passage reaction, the flow velocity of aluminium chloride is 3.00ml/min, and the flow velocity of sodium bicarbonate solution is 2.00ml/min, into anti-
It answers the aluminium chloride of device and sodium bicarbonate molar ratio is 0.48, reaction temperature is 15 DEG C, and the residence time is 5 minutes, obtained hydrogen-oxygen
Change aluminium suspension through filtration washing, separately weigh erythrosine solid 4.5g, pigment and chlorination al mole ratio are 0.05, and it is red to prepare 2%
Filter cake active aluminium hydroxide carrier is added in the solution of erythrosine by the red solution of moss, after being heated with stirring to 30 DEG C of abundant reactions
Filtering, filter cake is washed, and obtains erythrosine color lake, and measurement average grain diameter is 1.0 μm, pigment content 37.7%.
Comparative example 1:
Comparative example 1 is the stirring comparative example of the prior art:
Aluminium chloride and sodium bicarbonate are configured to solution respectively, 24.1g aluminium chlorohydrate is weighed and is configured to 500mL aqueous solution
(0.2mol/L) weighs 21g sodium bicarbonate and is configured to 400mL aqueous solution (0.62mol/L), by chlorination under the conditions of being stirred at room temperature
Aluminum solutions are slowly dropped in sodium bicarbonate solution, and the aluminum hydroxide precipitation of generation is filtered washing, separately weighs famille rose
Solid 3.0g, pigment and chlorination al mole ratio are 0.05, prepare 2% cochineal solution, filter cake active aluminium hydroxide carrier is added
Enter into carmine solution, agitating and heating filters after sufficiently reacting, and filter cake is washed, and obtains color lake, measures average grain
Diameter is 4 μm, pigment content 32.1%.
Comparative example 2:
Liquor alumini chloridi and sodium bicarbonate solution are prepared, 24.1g aluminium chlorohydrate is weighed and is configured to 500mL aqueous solution
(0.2mol/L) weighs 21g sodium bicarbonate and is configured to 800mL aqueous solution (0.62mol/L), and two kinds of materials are pumped by metering pump
Enter micro passage reaction, the flow velocity of aluminium chloride is 1.20ml/min, and the flow velocity of sodium bicarbonate solution is 0.60ml/min, into anti-
It answers the aluminium chloride of device and sodium bicarbonate molar ratio is 0.65, reaction temperature is 40 DEG C, and the residence time is 13.9 minutes, obtained hydrogen
Aluminium oxide suspension separately weighs carmine solid 3.0g through filtration washing, and pigment and chlorination al mole ratio are 0.05, prepares 2%
Filter cake active aluminium hydroxide carrier is added in carmine solution by cochineal solution, is heated with stirring to 30 DEG C of sufficiently reactions
After filter, filter cake is washed, obtains carmine lake, measurement average grain diameter is 2.7 μm, pigment content 33.6%.
By comparative example 1,2 and each embodiment it is found that the present invention is by largely groping and matching microchannel principle
Using, just obtain can making the partial size in color lake to be down to 1 μm of method of the invention below, the quality of the color lake Lai Tigao product, simultaneously
Keep the elution of chloride ion in final color lake product washing process more easy.
The present invention is based on principle be:
So far, there is not yet carrying out the technical study of color lake synthesis with microchannel continuous stream mode, the present invention provides
A method of edible color lake product is prepared using microchannel apparatus.
Micro passage reaction is a kind of continuous flow pipeline reactor, it is characterised in that line size is micro- between 10-1000
Between rice, the space of chemical reaction is controlled in small range, so that the distance of mass transfer greatly shortens, while increasing specific surface
Product, enables reaction mass to be quickly sufficiently mixed, and mass-transfer efficiency is much higher than agitating paddle used in common still reaction.Surface simultaneously
Long-pending increase makes the heat-transfer capability of reactor beyond traditional heat exchangers an order of magnitude.Continuous flow by microchannel is laminar flow shape
State, back-mixing effect is minimum, and the accurate control of reaction process may be implemented.
Applicant is to have passed through the application for largely groping and matching microchannel principle, just obtains that color lake can be made
Partial size is down to 1 μm or less this method, the quality of the color lake Lai Tigao product, while making chloride ion in final color lake product washing process
Elution it is more easy.
Claims (5)
1. preparing the method in small particle color lake in a kind of continuous flow micro passage reaction, which comprises the steps of:
Step 1: aluminium chloride and sodium bicarbonate solution are prepared, wherein the concentration of the liquor alumini chloridi is 0.3-0.8mol/L,
The concentration of the sodium bicarbonate solution is 0.1-0.2mol/L；
Step 2: liquor alumini chloridi and sodium bicarbonate solution are passed through in micro passage reaction by metering pump and carry out aluminium hydroxide
Carrier preparation reaction, coutroi velocity, keeps the aluminium chloride reacted and sodium bicarbonate molar ratio is 0.35-0.5, reaction temperature
It is 15-30 DEG C, residence time of the reaction solution in micro passage reaction is 60-600s, and it is outstanding that aluminium hydroxide is obtained after reflection
Aluminium hydroxide suspension filtration washing it is spare to be obtained active aluminium hydroxide by turbid；
Step 3: by the active aluminium hydroxide obtained in step 2, the mixed solution of synthetic food colors and aluminium chloride,
For secondary hybrid reaction to form color lake, secondary mixed reaction temperature is 10-40 DEG C；
Step 4: the color lake that step 3 obtains is carried out to obtain color lake product after chloride ion processing is dispelled in washing, wherein the color
The partial size of shallow lake product is less than 1.5 μm.
2. the method for preparing small particle color lake in a kind of continuous flow micro passage reaction as described in claim 1, feature exist
In the step one specifically: prepare aluminium chloride and sodium bicarbonate solution, weigh sodium bicarbonate solid, be dissolved in distilled water
In, being configured to concentration is 0.3-0.8mol/L solution, weighs aluminum chloride solids, is dissolved in distilled water, being configured to concentration is
The solution of 0.1-0.2mol/L.
3. the method for preparing small particle color lake in a kind of continuous flow micro passage reaction as described in claim 1, feature exist
In in the step 3, the synthetic food colors includes carmine, temptation red, sunset yellow, lemon yellow, brilliant blue, erythrosine
In any one or more.
4. the method for preparing small particle color lake in a kind of continuous flow micro passage reaction as described in claim 1, feature exist
In in the mixed solution of the synthetic food colors and aluminium chloride, the molar ratio of pigment used and raw material aluminium chloride is 0.04-
0.10。
5. the method for preparing small particle color lake in a kind of continuous flow micro passage reaction as described in claim 1, feature exist
In the partial size of the color lake product is less than 1 μm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811592470.6A CN109439018B (en) | 2018-12-25 | 2018-12-25 | Method for preparing small-particle-size lake in continuous-flow microchannel reactor |
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| CN201811592470.6A CN109439018B (en) | 2018-12-25 | 2018-12-25 | Method for preparing small-particle-size lake in continuous-flow microchannel reactor |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110354796A (en) * | 2019-07-31 | 2019-10-22 | 湖南雅城新材料有限公司 | A kind of aluminium salt type lithium adsorbent and the preparation method and application thereof |
| CN114410122A (en) * | 2021-12-23 | 2022-04-29 | 上海染料研究所有限公司 | Method for synthesizing tartrazine by micro-channel continuous flow and product thereof |
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| CN1515183A (en) * | 2003-08-27 | 2004-07-28 | 上海染料研究所有限公司 | Preparation method of edible color lake for special food additive |
| US20090139430A1 (en) * | 2007-11-30 | 2009-06-04 | Canon Kabushiki Kaisha | Method for manufacturing pigment dispersion |
| CN108504133A (en) * | 2018-05-09 | 2018-09-07 | 浙江大学 | A kind of nano particle and preparation method thereof of package natural pigment |
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2018
- 2018-12-25 CN CN201811592470.6A patent/CN109439018B/en active Active
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|---|---|---|---|---|
| CN1515183A (en) * | 2003-08-27 | 2004-07-28 | 上海染料研究所有限公司 | Preparation method of edible color lake for special food additive |
| US20090139430A1 (en) * | 2007-11-30 | 2009-06-04 | Canon Kabushiki Kaisha | Method for manufacturing pigment dispersion |
| CN108504133A (en) * | 2018-05-09 | 2018-09-07 | 浙江大学 | A kind of nano particle and preparation method thereof of package natural pigment |
Non-Patent Citations (1)
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| 闫士杰等: "微反应器构建、表征及其在染颜料中应用研究", 《染料与染色》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110354796A (en) * | 2019-07-31 | 2019-10-22 | 湖南雅城新材料有限公司 | A kind of aluminium salt type lithium adsorbent and the preparation method and application thereof |
| CN110354796B (en) * | 2019-07-31 | 2022-11-15 | 湖南雅城新能源股份有限公司 | Aluminum salt type lithium adsorbent and preparation method and application thereof |
| CN114410122A (en) * | 2021-12-23 | 2022-04-29 | 上海染料研究所有限公司 | Method for synthesizing tartrazine by micro-channel continuous flow and product thereof |
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