CN113277544B - Method for preparing color master batch by using dicyandiamide waste residues - Google Patents
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- C01F11/00—Compounds of calcium, strontium, or barium
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- C01F11/182—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by an additive other than CaCO3-seeds
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- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/18—Carbonates
- C01F11/182—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by an additive other than CaCO3-seeds
- C01F11/183—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by an additive other than CaCO3-seeds the additive being an organic compound
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Abstract
A method for preparing color master batches by utilizing dicyandiamide waste residues adopts dicyandiamide waste residue particles as a filler of the color master batches, and the method for preparing the dicyandiamide waste residue particles comprises the following steps: the method comprises the following steps: adding deionized water into the dicyandiamide waste residue to form a suspension; step two: introducing carbon dioxide gas into the suspension, then filtering, and taking supernatant to obtain first filter residue; step three: adding an emulsifier into the supernatant to prepare a first emulsion; step four: mixing the first emulsion with a second reagent, and then filtering to obtain a reactant; step five: drying the reactant to obtain the filler; the second reagent comprises calcium hydroxide. The method for preparing calcium carbonate as the filler by using the dicyandiamide waste residues has the advantages of high regeneration utilization rate of the dicyandiamide waste residues, low reagent consumption, simple process and low cost.
Description
Technical Field
The invention belongs to the technical field of industrial waste residue recycling, and particularly relates to a method for preparing color master batches by using dicyandiamide waste residues.
Background
Dicyandiamide is produced by lime nitrogen through hydrolysis, decalcification, polymerization, crystallization, filtration, drying and the like, and a large amount of waste residues are produced in the hydrolysis and decalcification stages. The main component of the dicyandiamide waste residue is calcium carbonate, the granularity of dry base residue (in an anhydrous state) is 0-0.1mm, and the dry base residue is gray black powder. At present, the stack of the dicyandiamide waste residues occupies a large amount of land. Due to drought, little rain and much wind in the north, the environment is easily polluted. In addition, dicyandiamide production enterprises need to pay a certain cost for treating waste residues, and the dicyandiamide waste residues become a bottleneck restricting the long-term development of dicyandiamide production enterprises. Dicyandiamide is the most important cyanamide product, and derivatives of dicyandiamide (such as imidazolidine and the like) are mainly used as intermediates for synthesizing pesticides and medicines, so that the demand for dicyandiamide products is extremely large. According to literature statistics, about five tons of dry residue are generated per ton of dicyandiamide produced. Therefore, the recycling of the dicyandiamide waste residue is a long-term research content.
At the present stage, the dicyandiamide waste residues are mainly used as cement additives, the use amount is small, the additional value is not high, and the calcium in the dicyandiamide waste residues is not well utilized.
Chinese patent No. CN103130428B discloses a method for producing lime by using dicyandiamide waste residue and carbide slag, which comprises mixing and stirring dicyandiamide waste residue and carbide slag, pressing and forming to obtain a blank, feeding the pressed blank into a carbonization kiln, introducing tail gas into the carbonization kiln for carbonization and drying, and feeding the carbonized and dried blank into a lime kiln for calcination to obtain lime. The method utilizes the dicyandiamide waste residue and the carbide slag to produce the lime with higher purity, but the method still stays in the coarse treatment stage of the dicyandiamide waste residue, and the application of utilizing the dicyandiamide waste residue to prepare the color master batch is not available at present.
In the application process of preparing the color master batch from the dicyandiamide waste residues, although calcium carbonate serving as a main component in the dicyandiamide waste residues can be used as a filler, the dicyandiamide waste residues are gray black, the process conditions for using the dicyandiamide waste residues as dark-color master batches (such as black, dark gray and the like) are simpler, and if the dicyandiamide waste residues are used as fillers of other light-color master batches, the color of the dicyandiamide waste residues interferes with the color formation of the color master batches, so that the application of the dicyandiamide waste residues in the field of preparing the color master batches is limited.
Disclosure of Invention
In view of the above problems, the present invention aims to provide a method for preparing color master batches from dicyandiamide waste residues, wherein the method for preparing calcium carbonate as a filler from dicyandiamide waste residues has the advantages of high regeneration utilization rate of dicyandiamide waste residues, low reagent consumption, simple process and low cost.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a method for preparing color master batches by utilizing dicyandiamide waste residues adopts dicyandiamide waste residue particles as a filler of the color master batches, and the method for preparing the dicyandiamide waste residue particles comprises the following steps: the method comprises the following steps: adding deionized water into the dicyandiamide waste residue to form a suspension; step two: introducing carbon dioxide gas into the suspension, then filtering, and taking supernatant to obtain first filter residue; step three: adding an emulsifier into the supernatant to prepare a first emulsion; step four: mixing the first emulsion with a second reagent, and then filtering to obtain a reactant; step five: drying the reactant to obtain the filler; the second reagent comprises calcium hydroxide.
The invention utilizes the dicyandiamide waste residue to prepare the light-colored filler, the main component of the filler is calcium carbonate, and the process flow hardly adds reagents such as acid, alkali and the like, thereby reducing the pollution.
As a further preferred aspect of the present invention, the method for preparing calcium hydroxide in the second reagent comprises: s1: adding an acidizing fluid into the first filter residue, and filtering to obtain a second filter residue and a mixed solution; s2: adding alkali liquor into the mixed solution, adjusting the pH range to be 4.0-5.0, and filtering to obtain a solution; s3: and continuously adding alkali liquor into the solution, adjusting the pH range to be 5.0-7.0, and filtering to obtain a calcium hydroxide solution.
In the invention, the waste residue generated in the process of preparing calcium carbonate, namely the first filter residue, is subjected to secondary utilization, and the product obtained by secondary utilization can be used as a raw material in the process of preparing calcium carbonate, so that the utilization rate of the dicyandiamide waste residue is further improved, and the production cost is saved.
As a further preferable mode of the invention, the solid-to-liquid ratio of the dicyandiamide waste residue to the deionized water in the first step is 1.
In a further preferred embodiment of the present invention, the temperature in the second step is 10 to 30 ℃.
As a further preferred aspect of the present invention, the emulsifier includes a nonionic surfactant and an auxiliary additive.
As a further preference of the invention, the non-ionic surfactant comprises one or more of Tween-20, tween-40, tween-60 and Tween-80.
As a further preferred of the present invention, the auxiliary additive comprises sodium oleate, stearic acid, sodium tripolyphosphate.
As a further preferred aspect of the present invention, the filler further includes a toner, and the toner is prepared by drying and pulverizing the second filter residue.
As a further preferred aspect of the present invention, the acidified liquid comprises hydrochloric acid.
As a further preference of the present invention, the lye comprises sodium hydroxide.
In conclusion, the invention has the following beneficial effects:
the light-colored filler is prepared by utilizing the dicyandiamide waste residues, so that the application range in the color master batch preparation field is widened; and the process flow hardly adds reagents such as acid, alkali and the like, thereby reducing the generation of pollution.
The waste residue generated in the process of preparing the filler is secondarily utilized, and the product obtained by secondary utilization, namely the calcium hydroxide, can be used as a raw material in the process of preparing the filler, so that the utilization rate of the waste residue of the dicyandiamide is further improved, and the production cost is saved.
In the preparation process of the invention, in which the calcium carbonate remained in the first filter residue is used as a supplementary raw material, the silicon dioxide and C existing in the first filter residue are directly separated and extracted, and can be used as a dyeing supplement prepared from dark master batches, thereby further improving the utilization rate of the dicyandiamide waste residues.
Detailed Description
The method for preparing the color master batch by using the dicyandiamide waste residue mainly comprises two process flows: the first is to utilize dicyandiamide offscum to prepare the filler of the light color, the principal ingredients of the filler are calcium carbonate, and reagents such as acid, alkali, etc. are hardly added to the technological process, have reduced the generating of the pollution; and secondly, waste residue generated in the process of preparing calcium carbonate, namely the first filter residue, is subjected to secondary utilization, and a product obtained by secondary utilization can be used as a raw material in the process of preparing calcium carbonate, so that the utilization rate of the dicyandiamide waste residue is further improved, and the production cost is saved.
In the invention, the process flow for preparing the light-color filler by using the dicyandiamide waste residue is shown in the attached figure 1 and comprises the following steps: the method comprises the following steps: adding deionized water into the dicyandiamide waste residue to form a suspension; step two: introducing carbon dioxide gas into the suspension, then filtering, and taking supernatant to obtain first filter residue; step three: adding an emulsifier into the supernatant to prepare a first emulsion; step four: mixing the first emulsion with a second reagent, and then filtering to obtain a reactant; step five: drying the reactant to obtain the filler; the second reagent comprises calcium hydroxide. In the invention, the main component of the second reagent is calcium hydroxide which can be directly purchased from the market, and the first filter residue generated in the process of preparing the filling agent can be further processed to prepare the calcium hydroxide.
In the present invention, the preparation method of calcium hydroxide in the second reagent comprises: s1: adding an acidizing fluid into the first filter residue, and filtering to obtain a second filter residue and a mixed solution; s2: adding alkali liquor into the mixed solution, adjusting the pH range to be 4.0-5.0, and filtering to obtain a solution; s3: and continuously adding alkali liquor into the solution, adjusting the pH range to be 5.0-7.0, and filtering to obtain a calcium hydroxide solution.
In the invention, the treatment method and the advantages of the dicyandiamide waste residue at least comprise the following steps: firstly, converting calcium carbonate with low solubility into calcium bicarbonate with high solubility by utilizing the principle that calcium carbonate in dicyandiamide is regressed into sodium bicarbonate after being introduced with excessive carbon dioxide, so as to achieve the purpose of separating the calcium carbonate from other impurity components such as ferric oxide, aluminum oxide, silicon dioxide, carbon monomer and the like in dicyandiamide waste residue; secondly, hydrochloric acid or other reagents in the traditional mode are not needed in the separation process, and deionized water is used as a solvent, so that the aim of separating calcium carbonate by a two-step method is fulfilled, the reagents are not needed to be consumed, and the production cost and the discharge cost are reduced; thirdly, adding an emulsifier into the obtained calcium bicarbonate solution to form a microemulsion structure, then adding another reactant calcium hydroxide microemulsion for mixing, and separating calcium ions, bicarbonate ions and hydroxyl ions from each other by a large amount of surfactant so as to regulate mass transfer among the ions, wherein the reaction is as follows:
fourthly, in the process of mixing and stirring the calcium hydroxide solution and the emulsifier to form the microemulsion, the surfactant can form a large amount of microemulsion micelles, so that the reaction speed is reduced, the growth of calcium carbonate crystal nuclei is inhibited, the particle size is effectively reduced, the calcium carbonate with smaller particle size and even reaching the nanometer level is applied as a filler of the color master, the dispersibility, the transparency and the glossiness are excellent, and the quality of the color master can be improved; fifthly, in the process of preparing the calcium bicarbonate solution from the dicyandiamide waste residues, because the solubility of calcium carbonate is low, part of calcium carbonate still exists in the first filter residue together with other components, at the moment, the residual calcium carbonate in the first filter residue is converted into calcium hydroxide by using an acid-base method, and the calcium hydroxide can be supplemented as a raw material for preparing nano-scale calcium carbonate; sixthly, in the preparation process of using the calcium carbonate remained in the first filter residue as a supplementary raw material, the silicon dioxide and C existing in the first filter residue are directly separated and extracted, and can be used as a coloring agent or a filling agent prepared from the dark master batch, so that the raw material is fully utilized.
In the first step, the solid-to-liquid ratio of the dicyandiamide waste residue to the deionized water is 1 to 20 to 100. In the invention, because the solubility of the calcium carbonate is low, excessive solvent, namely deionized water is needed to be adopted to dissolve the dicyandiamide waste residue, so that calcium carbonate is dissolved in water as much as possible, and in order to not introduce new ions, the adopted solvent is deionized water.
In the invention, the temperature in the second step is 10 to 30 ℃. The process of converting calcium carbonate into calcium bicarbonate is reversible, wherein the temperature is an important influence factor, so that the temperature needs to be controlled within the range of 10 to 30 ℃ in the process, and the conversion of calcium bicarbonate-calcium carbonate is reduced.
In the invention, the emulsifier comprises a nonionic surfactant and an auxiliary additive.
In the invention, the non-ionic surfactant comprises one or more of tween-20, tween-40, tween-60 and tween-80. Experiments prove that the layering occurrence rate of the Tween-80 in the process of preparing the emulsion is the minimum, so the Tween-80 is selected as the main emulsifier.
In the invention, the auxiliary additive comprises sodium oleate, stearic acid and sodium tripolyphosphate. The sodium oleate, the stearic acid and the sodium tripolyphosphate have the functions of assisting in forming the microemulsion and promoting the formation of the microemulsion.
In the invention, the filler further comprises a toner, and the toner is prepared by drying and crushing the second filter residue. The toner, namely the silicon dioxide and the C mentioned in the above, can be used as an auxiliary coloring agent of the dark master batch.
In the invention, the acidizing fluid comprises hydrochloric acid, and the alkali liquor comprises sodium hydroxide.
Example 1
Preparation of the first emulsion: (1) Taking 1kg of dicyandiamide waste residue, adding 50L of deionized water, stirring, introducing sufficient carbon dioxide at 20 ℃ until the conductivity of the mixed solution is not increased any more, filtering, and taking supernatant to obtain first filter residue; (2) Quantitatively measuring 1L of supernatant, adding 1L of tween-80, controlling the temperature at 25 ℃, stirring at the speed of 1000r/min for 15min, then adding 0.5g of sodium oleate, 5g of stearic acid and 0.2g of sodium tripolyphosphate, and continuously stirring for 10min to form a first emulsion.
Preparation of the second reagent: (1) mixing a mixture of 1g: dissolving the first filter residue in hydrochloric acid (0.31 mol/L) at a solid-to-liquid ratio of 50ml, adjusting the temperature to 35 ℃, stirring at a speed of 1000r/min, and performing suction filtration after 60min to obtain a second filter residue and a mixed solution; (2) Adding sodium hydroxide solution (1 mol/L) to adjust the pH value to be within the range of 4 to 5, and filtering the precipitated precipitate; (3) And continuously adding a sodium hydroxide solution to adjust the pH value to be within the range of 5 to 7, and filtering the precipitated precipitate to obtain a calcium hydroxide solution.
Preparation of calcium carbonate: dropwise adding a calcium hydroxide solution into the first emulsion at a speed of 3ml/min, stirring at a speed of 1000r/min, detecting the pH until the pH is about 7, and stopping dropwise adding; filtering, and drying in a 60 ℃ oven to obtain solid calcium carbonate.
Example 2
Preparation of the first emulsion: (1) Taking 1kg of dicyandiamide waste residue, adding 100L of deionized water, stirring, introducing sufficient carbon dioxide at 10 ℃ until the conductivity of the mixed solution is not increased any more, filtering, and taking supernatant to obtain first filter residue; (2) Quantitatively measuring 1L of supernatant, adding 2L of tween-80, controlling the temperature at 30 ℃, stirring at the speed of 800r/min for 20min, then adding 1.0g of sodium oleate, 5g of stearic acid and 0.2g of sodium tripolyphosphate, and continuously stirring for 20min to form a first emulsion.
Preparation of the second reagent: (1) mixing a mixture of 1g: dissolving the first filter residue in hydrochloric acid (0.31 mol/L) at a solid-to-liquid ratio of 50ml, adjusting the temperature to 30 ℃, stirring at a speed of 800r/min, and performing suction filtration after 60min to obtain a second filter residue and a mixed solution; (2) Adding a sodium hydroxide solution (1 mol/L) to adjust the pH value to be within a range of 4 to 5, and filtering a precipitated precipitate; (3) And continuously adding a sodium hydroxide solution to adjust the pH value to be within the range of 5 to 7, and filtering the precipitated precipitate to obtain a calcium hydroxide solution.
Preparation of calcium carbonate: dropwise adding a calcium hydroxide solution into the first emulsion at a speed of 5ml/min, stirring at a speed of 800r/min, detecting the pH until the pH is about 7, and stopping dropwise adding; filtering, and drying in a 60 ℃ oven to obtain solid calcium carbonate.
Example 3
Preparation of the first emulsion: (1) Taking 1kg of dicyandiamide waste residue, adding 50L of deionized water, stirring, introducing sufficient carbon dioxide at 30 ℃ until the conductivity of the mixed solution is not increased any more, filtering, and taking supernatant to obtain first filter residue; (2) Quantitatively measuring 1L of supernatant, adding 1.5L of Tween-80, controlling the temperature at 30 ℃, stirring at the speed of 1000r/min for 30min, then adding 0.5g of sodium oleate, 5g of stearic acid and 0.2g of sodium tripolyphosphate, and continuously stirring for 20min to form a first emulsion.
Preparation of the second reagent: (1) mixing 1g: dissolving the first filter residue in hydrochloric acid (0.31 mol/L) at a solid-to-liquid ratio of 50ml, adjusting the temperature to 30 ℃, stirring at a speed of 1000r/min, and performing suction filtration after 60min to obtain a second filter residue and a mixed solution; (2) Adding a sodium hydroxide solution (1 mol/L) to adjust the pH value to be within a range of 4 to 5, and filtering a precipitated precipitate; (3) And continuously adding a sodium hydroxide solution to adjust the pH value to be within the range of 5 to 7, and filtering the precipitated precipitate to obtain a calcium hydroxide solution.
Preparation of calcium carbonate: dropwise adding a calcium hydroxide solution into the first emulsion at a speed of 2ml/min, wherein the stirring speed is 800r/min, detecting the pH until the pH is about 7, and stopping dropwise adding; filtering, and drying in a 60 ℃ oven to obtain solid calcium carbonate.
Example 4
Preparation of the first emulsion: (1) Taking 1kg of dicyandiamide waste residue, adding 50L of deionized water, stirring, introducing sufficient carbon dioxide at 20 ℃ until the conductivity of the mixed solution is not increased any more, filtering, and taking supernatant to obtain first filter residue; (2) Quantitatively measuring 1L of supernatant, adding 1L of tween-80, controlling the temperature at 25 ℃, stirring at the speed of 1000r/min for 15min, then adding 0.5g of sodium oleate, 5g of stearic acid and 0.2g of sodium tripolyphosphate, and continuously stirring for 10min to form a first emulsion.
Preparation of the second reagent: a calcium hydroxide solution (3 g/100 ml) was prepared by dissolving commercially available calcium hydroxide powder in water.
Preparation of calcium carbonate: dropwise adding a calcium hydroxide solution into the first emulsion at a speed of 3ml/min, stirring at a speed of 1000r/min, detecting the pH until the pH is about 7, and stopping dropwise adding; filtering, and drying in a 60 ℃ oven to obtain solid calcium carbonate.
Comparative example 1
Commercially available calcium carbonate powder was purchased directly.
The solid calcium carbonate prepared in examples 1 to 4 and the calcium carbonate in comparative example 1 were measured, and the results were as follows:
the experimental data prove that the indexes of the calcium carbonate powder prepared by the invention are slightly inferior to those of commercial industrial calcium carbonate powder, but all the indexes meet the requirements of a color master batch filler, and the reason that the index of the example 4 is superior to that of the examples 1 to 3 is probably that the impurity content of the calcium hydroxide solution prepared from the first filter residue is still higher.
The specific embodiments described herein are merely illustrative of the spirit of the invention. Various modifications or additions may be made to the described embodiments, or alternatives may be employed, by those skilled in the art, without departing from the spirit or ambit of the invention as defined in the appended claims.
Claims (7)
1. A method for preparing color master batches by utilizing dicyandiamide waste residues is characterized in that dicyandiamide waste residue particles are used as a filler of the color master batches, and the method for preparing the dicyandiamide waste residue particles comprises the following steps:
the method comprises the following steps: adding deionized water into the dicyandiamide waste residue to form a suspension;
step two: introducing carbon dioxide gas into the suspension, then filtering, and taking supernatant to obtain first filter residue;
step three: adding an emulsifier into the supernatant to prepare a first emulsion;
step four: mixing the first emulsion with a second reagent, and then filtering to obtain a reactant;
step five: drying the reactant to obtain the filler;
the second reagent comprises calcium hydroxide;
the emulsifier comprises a nonionic surfactant and an auxiliary additive;
the non-ionic surfactant comprises one or more of tween-20, tween-40, tween-60 and tween-80;
the auxiliary additive comprises sodium oleate, stearic acid and sodium tripolyphosphate.
2. The method for preparing color master batches by using dicyandiamide waste residues as claimed in claim 1, wherein the method for preparing calcium hydroxide in the second reagent comprises the following steps:
s1: adding an acidizing fluid into the first filter residue, and filtering to obtain a second filter residue and a mixed solution;
s2: adding alkali liquor into the mixed solution, adjusting the pH range to be 4.0-5.0, and filtering to obtain a solution;
s3: and continuously adding alkali liquor into the solution, adjusting the pH range to be 5.0 to 7.0, and filtering to obtain a calcium hydroxide solution.
3. The method for preparing the color master batch from the dicyandiamide waste residue according to claim 1, wherein in the first step, the solid-to-liquid ratio of the dicyandiamide waste residue to deionized water is 1 to 20 to 100.
4. The method for preparing the color master batch from the dicyandiamide waste residue according to claim 1, wherein the temperature in the second step is 10 to 30 ℃.
5. The method for preparing color masterbatch by using dicyandiamide waste residue as claimed in claim 2, wherein the filler further comprises a toner, and the toner is prepared by drying and crushing the second filter residue.
6. The method for preparing color master batches by using dicyandiamide waste residues as claimed in claim 2, wherein the acidizing fluid comprises hydrochloric acid.
7. The method for preparing color master batches by using dicyandiamide waste residues as claimed in claim 2, wherein the alkali solution comprises sodium hydroxide.
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