CN109439018B - Method for preparing small-particle-size lake in continuous-flow microchannel reactor - Google Patents
Method for preparing small-particle-size lake in continuous-flow microchannel reactor Download PDFInfo
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- CN109439018B CN109439018B CN201811592470.6A CN201811592470A CN109439018B CN 109439018 B CN109439018 B CN 109439018B CN 201811592470 A CN201811592470 A CN 201811592470A CN 109439018 B CN109439018 B CN 109439018B
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- lake
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- sodium bicarbonate
- aluminum chloride
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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
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- Chemical Kinetics & Catalysis (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention discloses a method for preparing small-particle-size lake in a continuous flow microchannel reactor, which comprises the following steps of: the method comprises the following steps: preparing aluminum chloride and sodium bicarbonate solution; step two: introducing an aluminum chloride solution and a sodium bicarbonate solution into a microchannel reactor through a metering pump to perform aluminum hydroxide carrier preparation reaction, controlling the flow rate, the molar ratio of aluminum chloride to sodium bicarbonate, the reaction temperature and the residence time of a reaction solution in the microchannel reactor, obtaining an aluminum hydroxide suspension after the reaction is finished, and filtering and washing the aluminum hydroxide suspension to obtain active aluminum hydroxide for later use; step three: preparing a color lake; step four: removing chloride ions from the lake to obtain a lake product with the particle size of less than 1.5 mu m. The invention adjusts and strengthens the mixing effect through mass transfer strengthening of micro-channel equipment and a large number of experiments, thereby preparing the active aluminum hydroxide matrix with small grain diameter, and obtaining the lake with the grain diameter lower than 1 mu m through loading pigment.
Description
Technical Field
The invention belongs to the field of lake preparation, and particularly relates to a method for preparing small-particle-size lake in a continuous flow microchannel reactor.
Background
The lake is a water-insoluble pigment formed by precipitation of a soluble dye under an alkaline condition or combined with metal hydroxide, and has the advantages of water insolubility, pigment migration prevention, high safety and stability. The quality of the product of the color lake is greatly influenced by the particle size, and if an aluminum hydroxide carrier with smaller particle size is formed, the supported pigment is more excellent in uniformity and coloring effect, the specific surface area is increased, and the method is more favorable in the process of washing chloride ions in post-treatment.
The existing process for producing the aluminum hydroxide with smaller particle size is carried out in a reaction kettle, stirring and slow feeding are used for obtaining the aluminum hydroxide, the particle size of the aluminum hydroxide can reach 1-5 mu m, but the traditional kettle type reactor has the disadvantages of slow heat and mass transfer due to self limitation, so that the defects of overlong reaction retention time, larger back mixing, unstable reaction control and the like are caused.
Disclosure of Invention
In order to overcome the above-mentioned defects of the prior art, the present invention aims to provide a method for preparing small-particle size lakes in a continuous flow microchannel reactor, so as to reduce the particle size of the carrier and improve the product quality and production stability.
In order to realize one of the purposes of the invention, the adopted technical scheme is as follows:
a method for preparing a small particle size lake in a continuous flow microchannel reactor, comprising the steps of:
the method comprises the following steps: preparing an aluminum chloride solution and a sodium bicarbonate solution, wherein the concentration of the aluminum chloride solution is 0.3-0.8mol/L, and the concentration of the sodium bicarbonate solution is 0.1-0.2 mol/L;
step two: introducing an aluminum chloride solution and a sodium bicarbonate solution into a microchannel reactor through a metering pump to perform an aluminum hydroxide carrier preparation reaction, controlling the flow rate, keeping the molar ratio of the aluminum chloride and the sodium bicarbonate for the reaction at 0.35-0.5, the reaction temperature at 15-30 ℃, keeping the residence time of a reaction solution in the microchannel reactor at 60-600s, obtaining an aluminum hydroxide suspension after the reaction is finished, and filtering and washing the aluminum hydroxide suspension to obtain active aluminum hydroxide for later use;
step three: synthesizing the active aluminum hydroxide prepared in the second step into a mixed solution of an edible pigment and aluminum chloride, and carrying out secondary mixing reaction to form lake, wherein the reaction temperature of the secondary mixing is 10-40 ℃;
step four: washing the lake obtained in the step three to remove chloride ions to obtain a lake product, wherein the particle size of the lake product is less than 1.5 mu m.
In a preferred embodiment of the present invention, the first step is specifically: preparing aluminum chloride and sodium bicarbonate solution, weighing sodium bicarbonate solid, dissolving in distilled water to prepare 0.3-0.8mol/L solution, weighing aluminum chloride solid, dissolving in distilled water to prepare 0.1-0.2mol/L solution.
In a preferred embodiment of the present invention, the synthetic food color in step three comprises any one or more of carmine, allura red, sunset yellow, lemon yellow, brilliant blue and erythrosine.
In a preferred embodiment of the invention, the molar ratio of the pigment to the raw material aluminum chloride in the mixed solution of the synthetic food pigment and the aluminum chloride is 0.04-0.10.
In a preferred embodiment of the invention, the particle size of the lake product is less than 1 μm.
The main innovation points of the invention are as follows: the invention utilizes the mass transfer enhancement of the microchannel equipment, adjusts and enhances the mixing effect through a large number of experiments, thereby preparing the small-particle-size active aluminum hydroxide substrate by a method for obtaining a product with smaller particle size in the reaction, and can obtain the lake with the particle size of less than 1 mu m by loading pigment.
Detailed Description
The invention is further described with reference to the following examples:
example 1:
the microchannel device is FlowChemistry System of Vapourtec, aluminum chloride solution and sodium bicarbonate solution are respectively prepared, 24.1g of aluminum chlorohydrate is weighed to prepare 500mL of aqueous solution (0.2mol/L), 21g of sodium bicarbonate is weighed to prepare 400mL of aqueous solution (0.62mol/L), the two materials are pumped into a microchannel reactor through a metering pump, the flow rate of aluminum chloride is 2.78mL/min, the flow rate of sodium bicarbonate solution is 2.22mL/min, the molar ratio of aluminum chloride and sodium bicarbonate entering the reactor is 0.4, the reaction temperature is 25 ℃, the retention time is 5 minutes, the obtained aluminum hydroxide suspension is filtered and washed, 3.0g of carmine solid is additionally weighed, the molar ratio of pigment to aluminum chloride is 0.05, 2% carmine solution is prepared, a filter cake active aluminum hydroxide carrier is added into the carmine solution, the mixture is stirred and heated to 40 ℃ for full reaction, the filter cake is washed, a carmine lake was obtained with a mean particle size of 1.1 μm and a pigment content of 36.1%.
Example 2:
preparing an aluminum chloride solution and a sodium bicarbonate solution according to the conditions and steps of example 1, pumping the two materials into a microchannel reactor through a metering pump, wherein the flow rate of aluminum chloride is 4.63ml/min, the flow rate of the sodium bicarbonate solution is 3.70ml/min, the molar ratio of the aluminum chloride to the sodium bicarbonate entering the reactor is 0.4, the reaction temperature is 25 ℃, the retention time is 3 minutes, filtering and washing the obtained aluminum hydroxide suspension, weighing 3.0g of cochineal solid, the molar ratio of the pigment to the aluminum chloride is 0.05, preparing a 2% carmine solution, adding a filter cake active aluminum hydroxide carrier into the carmine solution, stirring and heating to 30 ℃, fully reacting, filtering, washing the filter cake to obtain carmine lake, measuring the average particle size to be 0.9 mu m, and the pigment content to be 38.3%.
Example 3:
preparing an aluminum chloride solution and a sodium bicarbonate solution according to the conditions and steps of example 1, pumping the two materials into a microchannel reactor through a metering pump, wherein the flow rate of aluminum chloride is 4.63ml/min, the flow rate of the sodium bicarbonate solution is 3.70ml/min, the molar ratio of the aluminum chloride to the sodium bicarbonate entering the reactor is 0.4, the reaction temperature is 30 ℃, the retention time is 3 minutes, filtering and washing the obtained aluminum hydroxide suspension, weighing 5.4g of sunset yellow solid, the molar ratio of pigment to the aluminum chloride is 0.12, preparing a 2% sunset yellow solution, adding a filter cake active aluminum hydroxide carrier into the sunset yellow solution, stirring and fully reacting at the temperature of 15 ℃, filtering, washing the filter cake to obtain sunset yellow precipitate, wherein the measured average particle size is 0.9 mu m, and the pigment content is 37.5%.
Example 4:
preparing an aluminum chloride solution and a sodium bicarbonate solution, weighing 24.1g of aluminum chlorohydrate to prepare 500mL of aqueous solution (0.2mol/L), weighing 23g of sodium bicarbonate to prepare 400mL of aqueous solution (0.55mol/L), pumping the two materials into a microchannel reactor through a metering pump, controlling the flow rate of aluminum chloride to be 2.78mL/min, controlling the flow rate of sodium bicarbonate solution to be 2.22mL/min, controlling the molar ratio of aluminum chloride to sodium bicarbonate to be 0.35, controlling the reaction temperature to be 20 ℃, controlling the retention time to be 5 minutes, filtering and washing the obtained aluminum hydroxide suspension, weighing 3.1g of lemon yellow solid and 0.058 of molar ratio of pigment to aluminum chloride, preparing a 2% lemon yellow solution, adding a filter cake active aluminum hydroxide carrier into the lemon yellow solution, stirring at the room temperature of 25 ℃, fully reacting, filtering, washing the filter cake to obtain the lemon yellow precipitate, measuring the average particle size to be 0.9 mu m, the pigment content was 36.8%.
Example 5:
preparing an aluminum chloride solution and a sodium bicarbonate solution, weighing 24.1g of aluminum chlorohydrate to prepare 1000mL of aqueous solution (0.1mol/L), weighing 23g of sodium bicarbonate to prepare 800mL of aqueous solution (0.55mol/L), pumping the two materials into a microchannel reactor through a metering pump, controlling the flow rate of aluminum chloride to be 15.0mL/min, controlling the flow rate of sodium bicarbonate solution to be 10.0mL/min, controlling the molar ratio of aluminum chloride to sodium bicarbonate to be 0.5, controlling the reaction temperature to be 15 ℃, controlling the retention time to be 1 min, filtering and washing the obtained aluminum hydroxide suspension, weighing 3.0g of allura red solid and controlling the molar ratio of a pigment to aluminum chloride to be 0.06, preparing a 2% allura red solution, adding a filter cake active aluminum hydroxide carrier into the allura red solution, stirring and heating to 35 ℃ for full reaction, filtering, washing the filter cake to obtain the allura red lake, measuring the average particle size to be 1.2 mu m, the pigment content was 34.9%.
Example 6:
preparing an aluminum chloride solution and a sodium bicarbonate solution, weighing 24.1g of aluminum chlorohydrate to prepare 500mL of aqueous solution (0.2mol/L), weighing 21g of sodium bicarbonate to prepare 800mL of aqueous solution (0.62mol/L), pumping the two materials into a microchannel reactor through a metering pump, controlling the flow rate of aluminum chloride to be 1.39mL/min and the flow rate of sodium bicarbonate solution to be 1.11mL/min, controlling the molar ratio of aluminum chloride to sodium bicarbonate to be 0.4, controlling the reaction temperature to be 15 ℃ and the retention time to be 10 minutes, filtering and washing the obtained aluminum hydroxide suspension, weighing 6.3g of brilliant blue solid and 0.08 mol ratio of pigment to aluminum chloride, preparing 2% brilliant blue solution, adding a filter cake active aluminum hydroxide carrier into the brilliant blue solution, stirring and heating to 40 ℃, fully reacting, filtering, washing the filter cake to obtain brilliant blue lake, measuring the average particle size to be 1.4 mu m, the pigment content was 38.7%.
Example 7:
preparing an aluminum chloride solution and a sodium bicarbonate solution, weighing 24.1g of aluminum chlorohydrate to prepare 500mL of an aqueous solution (0.2mol/L), weighing 21g of sodium bicarbonate to prepare 800mL of an aqueous solution (0.62mol/L), pumping the two materials into a microchannel reactor through a metering pump, controlling the flow rate of aluminum chloride to be 3.00mL/min and the flow rate of the sodium bicarbonate solution to be 2.00mL/min, controlling the molar ratio of aluminum chloride to sodium bicarbonate entering the reactor to be 0.48, controlling the reaction temperature to be 15 ℃ and the retention time to be 5 minutes, filtering and washing the obtained aluminum hydroxide suspension, weighing 4.5g of erythrosine solid and controlling the molar ratio of pigment to aluminum chloride to be 0.05, preparing a 2% erythrosine solution, adding a filter cake active aluminum hydroxide carrier into the erythrosine solution, stirring and heating to 30 ℃, fully reacting, filtering, washing the filter cake to obtain erythrosine lake, measuring the average particle size to be 1.0 mu m, the pigment content was 37.7%.
Comparative example 1:
comparative example 1 is a prior art stirring comparative example:
respectively preparing aluminum chloride and sodium bicarbonate into solutions, weighing 24.1g of aluminum chlorohydrate to prepare 500mL of aqueous solution (0.2mol/L), weighing 21g of sodium bicarbonate to prepare 400mL of aqueous solution (0.62mol/L), slowly dripping the aluminum chloride solution into the sodium bicarbonate solution under the condition of stirring at room temperature, filtering and washing the generated aluminum hydroxide precipitate, weighing 3.0g of carmine solid, wherein the molar ratio of pigment to aluminum chloride is 0.05, preparing 2% carmine solution, adding a filter cake active aluminum hydroxide carrier into the carmine solution, stirring, heating, fully reacting, filtering, washing a filter cake to obtain a lake, wherein the measured average particle size is 4 mu m, and the pigment content is 32.1%.
Comparative example 2:
preparing an aluminum chloride solution and a sodium bicarbonate solution, weighing 24.1g of aluminum chlorohydrate to prepare 500mL of an aqueous solution (0.2mol/L), weighing 21g of sodium bicarbonate to prepare 800mL of an aqueous solution (0.62mol/L), pumping the two materials into a microchannel reactor through a metering pump, controlling the flow rate of aluminum chloride to be 1.20mL/min and the flow rate of sodium bicarbonate solution to be 0.60mL/min, controlling the molar ratio of aluminum chloride to sodium bicarbonate to be 0.65, controlling the reaction temperature to be 40 ℃ and the retention time to be 13.9 minutes, filtering and washing the obtained aluminum hydroxide suspension, weighing 3.0g of carmine solid and 0.05 molar ratio of pigment to aluminum chloride, preparing a 2% carmine solution, adding a filter cake active aluminum hydroxide carrier into the carmine solution, stirring and heating to 30 ℃ for full reaction, filtering, washing the filter cake to obtain carmine lake, measuring the average particle size to be 2.7 mu m, the pigment content was 33.6%.
As can be seen from comparative examples 1 and 2 and examples, the present invention, through the extensive exploration and application of the principles of the microchannel technology, resulted in the method of the present invention which allows the particle size of the lake to be reduced to below 1 μm, to improve the quality of the lake product, and to facilitate the elution of chloride ions during the final wash of the lake product.
The principle on which the invention is based is that:
to date, no process study has been found for lake synthesis using microchannel continuous flow, and the present invention provides a process for preparing an edible lake product using microchannel apparatus.
The microchannel reactor is a continuous flow pipeline type reactor, and is characterized in that the size of a pipeline is between 10 and 1000 micrometers, the space of chemical reaction is controlled in a tiny range, the distance of mass transfer is greatly shortened, the specific surface area is increased, reaction materials can be quickly and fully mixed, and the mass transfer efficiency is far higher than that of a stirring paddle used in the common kettle type reaction. At the same time, the increase in surface area makes the heat transfer capacity of the reactor an order of magnitude greater than that of conventional heat exchangers. The continuous flow passing through the microchannel is in a laminar flow state, the back mixing effect is extremely small, and the precise control of the reaction process can be realized.
The applicant obtains the method which can reduce the grain size of the lake to be less than 1 mu m through a large amount of research and application of matching microchannel technical principle, so as to improve the quality of the lake product and simultaneously facilitate the elution of chloride ions in the washing process of the final lake product.
Claims (4)
1. A method for preparing a small particle size lake in a continuous flow microchannel reactor, comprising the steps of:
the method comprises the following steps: preparing an aluminum chloride solution and a sodium bicarbonate solution, wherein the concentration of the aluminum chloride solution is 0.3-0.8mol/L, and the concentration of the sodium bicarbonate solution is 0.1-0.2 mol/L;
step two: introducing an aluminum chloride solution and a sodium bicarbonate solution into a microchannel reactor through a metering pump to perform an aluminum hydroxide carrier preparation reaction, controlling the flow rate, keeping the molar ratio of the aluminum chloride and the sodium bicarbonate for the reaction at 0.35-0.5, the reaction temperature at 15-30 ℃, keeping the residence time of a reaction solution in the microchannel reactor at 60-600s, obtaining an aluminum hydroxide suspension after the reaction is finished, and filtering and washing the aluminum hydroxide suspension to obtain active aluminum hydroxide for later use;
step three: synthesizing the active aluminum hydroxide prepared in the second step into a mixed solution of an edible pigment and aluminum chloride, and carrying out secondary mixing reaction to form lake, wherein the reaction temperature of the secondary mixing is 10-40 ℃;
step four: washing the lake obtained in the step three to remove chloride ions to obtain a lake product, wherein the particle size of the lake product is less than 1.5 mu m;
the microchannel apparatus is a flowchemistry system from Vapourtec.
2. The method of claim 1, wherein in step three, the synthetic food color comprises any one or more of carmine, allura red, sunset yellow, lemon yellow, brilliant blue, and erythrosine.
3. The process of claim 1, wherein the pigment to aluminum chloride is used in a molar ratio of 0.04 to 0.10 in the mixed solution of synthetic food pigment and aluminum chloride.
4. The process for the preparation of small particle size lakes in a continuous flow microchannel reactor of claim 1, wherein the size of the lake product is less than 1 μm.
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