CN112250976A - High-concentration ammonia-removing color cake and application thereof - Google Patents
High-concentration ammonia-removing color cake and application thereof Download PDFInfo
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Abstract
The invention discloses a high-concentration ammonia color removal cake which comprises the following raw materials in percentage by weight: 10-15% of PVB, 15-20% of plasticizer, 2-3% of coupling agent, 3-4% of toughening agent, 0.5-1.5% of lubricant and 60-65% of ammonia removal auxiliary agent; the ammonia removal auxiliary agent comprises the following raw materials in percentage by weight: 20% of aluminum chloride, 60% of aluminum metaphosphate and 20% of citric acid. The invention improves the compatibility among the components through the mutual synergy among the components, and ensures that the prepared ammonia removal color cake has higher concentration.
Description
Technical Field
The invention relates to the technical field of ammonia removal of foaming agents, in particular to a high-concentration ammonia removal color cake and application thereof.
Background
The azodicarbonamide foaming agent is yellow solid powder, and the azodicarbonamide occupies more than 80% of the foaming agent market at present due to large gas production and high cost performance. However, in the decomposition process of the common azodicarbonamide foaming agent, a byproduct ammonia gas is generated, the ammonia gas is an inorganic compound, is gas at normal temperature, is colorless and has irritant odor, the content of the ammonia gas is too high, the human health is influenced, in recent years, along with the enhancement of environmental awareness of consumers, the environmental protection and export standards are stricter and stricter, and the application field of the azodicarbonamide foaming agent is limited due to the irritant odor.
At present, some ammonia removers are added into foaming products to achieve the effect of removing ammonia gas, the adding amount of the ammonia removers needs to be large to achieve a good ammonia removing effect, and the large amount of the ammonia removers is added to cause poor compatibility of the ammonia removers and foaming product raw materials, so that the raw materials and the ammonia removers are separated out, and the product quality is influenced.
Disclosure of Invention
In view of the prior art, the invention aims to provide a high-concentration ammonia removal color cake, PVB is used as a carrier, the types and the use amounts of a plasticizer, a coupling agent, a toughening agent, a lubricant and an ammonia removal auxiliary agent are reasonably controlled, and the compatibility among all components is improved through the mutual cooperation among all the components, so that the concentration of the prepared ammonia removal color cake is higher.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect of the invention, a high-concentration ammonia-removing color cake is provided, which comprises the following raw materials in percentage by weight: 10-15% of PVB, 15-20% of plasticizer, 2-3% of coupling agent, 3-4% of toughening agent, 0.5-1.5% of lubricant and 60-65% of ammonia removal auxiliary agent; the ammonia removal auxiliary agent comprises the following raw materials in percentage by weight: 20% of aluminum chloride, 60% of aluminum metaphosphate and 20% of citric acid.
Preferably, the plasticizer is prepared by the following preparation method: (1) distilling the residual ethylene glycol liquid at the temperature of 140 ℃ and 150 ℃ for 1-2h to obtain high-concentration ethylene glycol liquid;
(2) mixing the high-concentration ethylene glycol raffinate obtained in the step (1) with caprylic-capric acid, and performing reflux reaction at 180-200 ℃ by using tetrabutyl titanate as a catalyst to prepare a plasticizer; the mass ratio of the high-concentration ethylene glycol raffinate to the caprylic-capric acid is 1:2, and the tetrabutyl titanate accounts for 2% of the total mass of the high-concentration ethylene glycol raffinate and the caprylic-capric acid.
According to the invention, high-yield ethylene glycol dicaprylic decanoate is obtained at a specific temperature by adopting a specific type of acid and a catalyst in combination with a proper amount; through research, the types and the dosage of acid and catalyst, and the temperature and the time of reaction have the function of mutual synergistic promotion, and the above parameters are all integral.
Preferably, in the step (1), the concentration of the ethylene glycol in the high-concentration ethylene glycol raffinate is 90%.
Preferably, in the step (2), the reflux reaction time is 5-6h, stirring is carried out during the reflux reaction, and the stirring speed is 80-90 r/min.
Preferably, in the step (2), the caprylic acid and the capric acid in the caprylic-capric acid are 30% and 70%.
Preferably, the coupling agent is a monoalkoxy pyrophosphate titanate coupling agent.
Preferably, the toughening agent is an ethylene-vinyl acetate copolymer.
Preferably, the lubricant is calcium stearate.
In a second aspect of the present invention, a method for preparing the high-concentration ammonia-removing color cake comprises the following steps: (1) plasticizing: the raw materials are put into an internal mixer for plasticizing and melting to obtain a plasticized melt, the temperature is 120-;
(2) grinding: grinding the plasticized melt obtained in the step (1) for 2-3 times by a three-roll grinder, wherein the grinding temperature is 90-100 ℃, each time is 15-20min, and the pressure is 5-10 kg;
(3) molding: tabletting and forming by a three-roller open mill at 40-50 ℃.
In a third aspect of the present invention, there is provided a use of the high-concentration ammonia removal color cake described above for removing ammonia from a PVB foamed product.
In the fourth aspect of the invention, a method for removing ammonia by using a high-concentration ammonia color removal cake is provided, wherein the high-concentration ammonia color removal cake is added into raw materials for preparing a PVB foamed product and is uniformly mixed with the raw materials, and the ratio of the use amount of the high-concentration ammonia color removal cake to the use amount of a foaming agent in the raw materials for the PVB foamed product is (0.5-1): 1.
the invention has the beneficial effects that:
1. the PVB is used as a carrier, the types and the amounts of the plasticizer, the coupling agent, the toughening agent, the lubricant and the ammonia removal auxiliary agent are reasonably controlled, and the compatibility among the components is improved through the mutual cooperation among the components, so that the concentration of the prepared ammonia removal color cake is higher.
2. When the high-concentration ammonia removal color cake prepared by the method is added into a PVB foaming product, the ammonia removal color cake is high in concentration, so that the adding amount is small, and meanwhile, the compatibility of each component of the high-concentration ammonia removal color cake is good, so that the compatibility of the components in the PVB foaming product is not poor, the precipitation of the components is avoided, and the product quality is ensured.
3. The plasticizer prepared by the method is ethylene glycol dicaprylate and ethylene glycol dicaprate, so that on one hand, the compatibility of the ammonia removal aid aluminum chloride, aluminum metaphosphate, citric acid and PVB can be obviously improved, the ammonia removal aid is prevented from being separated out, and the high-concentration addition amount of the ammonia removal aid is realized; the dosage of the ammonia removal additive can reach 60-65%, and the ammonia removal additive can not be separated out, so that a high-concentration ammonia removal color cake can be obtained, and the ammonia removal effect in a PVB foaming product is ensured; on the other hand, the invention reuses the glycol raffinate generated in the dioctyl terephthalate (DOTP) production process as the preparation of the plasticizer, thereby improving the utilization value of the glycol raffinate and the economic benefit; the low-value ethylene glycol raffinate is converted into the high-value plasticizer, so that the production cost is greatly reduced.
4. The invention realizes better ammonia removal effect by reasonably controlling the types and the dosage of all components in the ammonia removal auxiliary agent; the citric acid in the ammonia removal auxiliary agent plays a role in guiding and catalyzing, and is combined with the foaming agent to inhibit the foaming agent from generating ammonia gas; the aluminum metaphosphate and the aluminum chloride are matched to realize the function of absorbing ammonia gas, and the aluminum chloride, the aluminum metaphosphate and the citric acid are matched with each other to realize synergistic interaction and avoid the generation of ammonia gas; the dosage of each component of the ammonia removal auxiliary agent is reasonably controlled, the effect of inhibiting ammonia gas is poor when the dosage is too small, and the components are easy to separate out when the dosage is too large.
Drawings
FIG. 1 is a gas chromatogram of the plasticizer produced from ethylene glycol raffinate and octyl-decyl acid.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the disclosure. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
The 'ethylene glycol raffinate' in the invention is a byproduct generated in the process of producing dioctyl terephthalate (DOTP). The method specifically comprises the following steps: polyethylene terephthalate (PET) is ethylene glycol which is separated in the esterification process under the high-temperature reaction of octanol and tetrabutyl titanate. The content of glycol in the residual glycol liquid is more than or equal to 43 percent.
As introduced in the background technology, in the decomposition process of the prior common azodicarbonamide foaming agent, a byproduct ammonia gas is generated, some ammonia removing agents are generated, the ammonia removing agents are added into a foaming product to achieve the effect of removing the ammonia gas, the adding amount of the ammonia removing agents needs to be large to achieve a good ammonia removing effect, and the ammonia removing agents are poor in compatibility with foaming product raw materials due to the large amount of the ammonia removing agents, so that the raw materials and the ammonia removing agents are separated out, and the product quality is influenced.
Based on the above, the invention discloses a high-concentration ammonia removal color cake, the PVB is used as a carrier, the types and the dosage of a plasticizer, a coupling agent, a toughening agent, a lubricant and an ammonia removal auxiliary agent are reasonably controlled, and the compatibility among the components is improved through the mutual cooperation among the components, so that the concentration of the prepared ammonia removal color cake is higher.
In the preparation process of the plasticizer, the reaction of the caprylic-capric acid and the glycol in the glycol raffinate is as follows:
HO-CH2-CH2-OH+2C7H15COOH→C7H15COO-CH2-CH2-OOC-C7H15+2H2O
HO-CH2-CH2-OH+2C9H19COOH→C9H19COO-CH2-CH2-OOC-C9H19+2H2O
the sources of the octyl and decyl mixed acid are wide, the cost performance is high, and the plasticizer product prepared by the reaction of the octyl and decyl mixed acid has good compatibility with PVB; if replaced by other acids, they have poor compatibility with PVB and the resulting products are prone to oil bleeding. In the reaction process, 180-phase reflux reaction at 200 ℃ is adopted, and when the temperature is too high, the octyl and decyl acid can be volatilized, and simultaneously, the ethylene glycol can be dehydrated to generate ether and aldehyde, so that the yield of the plasticizer is influenced.
In order to make the technical solutions of the present application more clearly understood by those skilled in the art, the technical solutions of the present application will be described in detail below with reference to specific embodiments.
The test materials used in the examples of the present invention are all conventional in the art and commercially available.
Example 1: the high-concentration ammonia-removing color cake comprises the following raw materials in percentage by weight: 15% of PVB, 15% of plasticizer, 2.5% of monoalkoxy pyrophosphate titanate coupling agent, 3% of ethylene-vinyl acetate copolymer, 0.5% of lubricant and 64% of ammonia removal auxiliary agent; the ammonia removal auxiliary agent comprises the following raw materials in percentage by weight: 20% of aluminum chloride, 60% of aluminum metaphosphate and 20% of citric acid.
The plasticizer is prepared by the following preparation method: (1) distilling the residual ethylene glycol liquid at the temperature of 140 ℃ for 2h to obtain high-concentration residual ethylene glycol liquid; the concentration of the ethylene glycol in the high-concentration ethylene glycol raffinate is 90 percent;
(2) mixing the high-concentration ethylene glycol raffinate obtained in the step (1) with caprylic-capric acid, and performing reflux reaction at 180 ℃ by using tetrabutyl titanate as a catalyst to prepare a plasticizer; the mass ratio of the high-concentration ethylene glycol raffinate to the caprylic-capric acid is 1:2, and the tetrabutyl titanate accounts for 2% of the total mass of the high-concentration ethylene glycol raffinate and the caprylic-capric acid; the reflux reaction time is 6h, stirring is carried out in the reflux reaction process, and the stirring speed is 80 r/min; the content of caprylic acid and capric acid in the caprylic-capric acid is 30 percent and 70 percent respectively.
The preparation method of the high-concentration ammonia-removing color cake comprises the following steps: (1) plasticizing: putting the raw materials into an internal mixer for plasticizing and melting to obtain a plasticized melt, wherein the temperature is 120 ℃, and the time is 1 h;
(2) grinding: grinding the plasticized melt obtained in the step (1) for 2 times by a three-roll grinder, wherein the grinding temperature is 100 ℃, each time is 15min, and the pressure is 10 kg;
(3) molding: tabletting and forming are carried out by a three-roller open mill, and the forming temperature is 40 ℃.
Example 2: the high-concentration ammonia-removing color cake comprises the following raw materials in percentage by weight: 10% of PVB, 20% of plasticizer, 2% of monoalkoxy pyrophosphate titanate coupling agent, 4% of ethylene-vinyl acetate copolymer, 1% of lubricant and 63% of ammonia removal auxiliary agent; the ammonia removal auxiliary agent comprises the following raw materials in percentage by weight: 20% of aluminum chloride, 60% of aluminum metaphosphate and 20% of citric acid.
The plasticizer is prepared by the following preparation method: (1) distilling the residual ethylene glycol liquid at the temperature of 150 ℃ for 1h to obtain high-concentration residual ethylene glycol liquid; the concentration of the ethylene glycol in the high-concentration ethylene glycol raffinate is 90 percent;
(2) mixing the high-concentration ethylene glycol raffinate obtained in the step (1) with caprylic-capric acid, and performing reflux reaction at 200 ℃ by using tetrabutyl titanate as a catalyst to prepare a plasticizer; the mass ratio of the high-concentration ethylene glycol raffinate to the caprylic-capric acid is 1:2, and the tetrabutyl titanate accounts for 2% of the total mass of the high-concentration ethylene glycol raffinate and the caprylic-capric acid; the reflux reaction time is 5-6h, stirring is carried out in the reflux reaction process, and the stirring speed is 90 r/min; the content of caprylic acid and capric acid in the caprylic-capric acid is 30 percent and 70 percent respectively.
The preparation method of the high-concentration ammonia-removing color cake comprises the following steps: (1) plasticizing: putting the raw materials into an internal mixer for plasticizing and melting to obtain a plasticized melt, wherein the temperature is 130 ℃, and the time is 1 h;
(2) grinding: grinding the plasticized melt obtained in the step (1) for 3 times by a three-roll grinder, wherein the grinding temperature is 90 ℃, the grinding time is 20min each time, and the pressure is 5 kg;
(3) molding: tabletting and forming are carried out by a three-roller open mill, and the forming temperature is 50 ℃.
Example 3: the high-concentration ammonia-removing color cake comprises the following raw materials in percentage by weight: 12% of PVB, 16% of plasticizer, 3% of monoalkoxy pyrophosphate titanate coupling agent, 3% of ethylene-vinyl acetate copolymer, 1.5% of lubricant and 64.5% of ammonia removal auxiliary agent; the ammonia removal auxiliary agent comprises the following raw materials in percentage by weight: 20% of aluminum chloride, 60% of aluminum metaphosphate and 20% of citric acid.
The plasticizer is prepared by the following preparation method: (1) distilling the residual ethylene glycol liquid at 145 ℃ for 1.5h to obtain high-concentration residual ethylene glycol liquid; the concentration of the ethylene glycol in the high-concentration ethylene glycol raffinate is 90 percent;
(2) mixing the high-concentration ethylene glycol raffinate obtained in the step (1) with caprylic-capric acid, and performing reflux reaction at 190 ℃ by using tetrabutyl titanate as a catalyst to prepare a plasticizer; the mass ratio of the high-concentration ethylene glycol raffinate to the caprylic-capric acid is 1:2, and the tetrabutyl titanate accounts for 2% of the total mass of the high-concentration ethylene glycol raffinate and the caprylic-capric acid; the reflux reaction time is 5.5h, stirring is carried out in the reflux reaction process, and the stirring rotating speed is 80 r/min; the content of caprylic acid and capric acid in the caprylic-capric acid is 30 percent and 70 percent respectively.
The preparation method of the high-concentration ammonia-removing color cake comprises the following steps: (1) plasticizing: putting the raw materials into an internal mixer for plasticizing and melting to obtain a plasticized melt, wherein the temperature is 125 ℃, and the time is 1 h;
(2) grinding: grinding the plasticized melt obtained in the step (1) for 2-3 times by a three-roll grinder, wherein the grinding temperature is 95 ℃, each time lasts for 15min, and the pressure is 8 kg;
(3) molding: tabletting and forming are carried out by a three-roller open mill, and the forming temperature is 45 ℃.
Comparative experiment
The high-concentration ammonia removal color cakes prepared in the embodiments 1-3 of the invention are respectively added into PVB foaming products, which are marked as the embodiment 1 group, the embodiment 2 group and the embodiment 3 group, wherein the adding amount of the high-concentration ammonia removal color cakes accounts for 60 percent of the amount of a raw material foaming agent of the PVB foaming products; the PVB foaming products without the high-concentration ammonia color removal cakes are used as a control group, the group 1, the group 2, the group 3 and the control group are respectively placed into a 1L open bottle, then each open bottle is respectively placed into an oven to be heated, the heating temperature of each oven is 80 ℃, and the heating time is 1 h. After the heating is finished, the odor grade of each oven is judged by an odor grade judge. Meanwhile, phenolphthalein test papers were placed in the open bottles of the group of example 1, the group of example 2, the group of example 3, and the control group, respectively, and it was checked whether the phenolphthalein test paper turned red.
The odor grade evaluation adopts the test standards of odor in the industry, and the grade test standards are as follows:
level 1: has no odor
And 2, stage: has slight odor, but no interference
And 3, level: has obvious smell and no interference
4, level: has higher strength
And 5, stage: the strength is very high
And 6, level: is difficult to bear
The odor rating results for the example 1, example 2, example 3 and control groups were as follows: the example 1 group was grade 2, the example 2 group and the example 3 group were grade 3, and the control group was grade 6.
The phenolphthalein test paper color development results of the example 1 group, the example 2 group, the example 3 group and the control group are as follows: the phenolphthalein test strips of the example 1 group, the example 2 group, and the example 3 group did not turn red, and the phenolphthalein test strip of the control group turned red.
The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims (9)
1. The high-concentration ammonia-removing color cake is characterized by comprising the following raw materials in percentage by weight: 10-15% of PVB, 15-20% of plasticizer, 2-3% of coupling agent, 3-4% of toughening agent, 0.5-1.5% of lubricant and 60-65% of ammonia removal auxiliary agent; the ammonia removal auxiliary agent comprises the following raw materials in percentage by weight: 20% of aluminum chloride, 60% of aluminum metaphosphate and 20% of citric acid.
2. The high-concentration ammonia color removal cake as claimed in claim 1, wherein the plasticizer is prepared by the following preparation method: (1) distilling the residual ethylene glycol liquid at the temperature of 140 ℃ and 150 ℃ for 1-2h to obtain high-concentration ethylene glycol liquid;
(2) mixing the high-concentration ethylene glycol raffinate obtained in the step (1) with caprylic-capric acid, and performing reflux reaction at 180-200 ℃ by using tetrabutyl titanate as a catalyst to prepare a plasticizer; the mass ratio of the high-concentration ethylene glycol raffinate to the caprylic-capric acid is 1:2, and the tetrabutyl titanate accounts for 2% of the total mass of the high-concentration ethylene glycol raffinate and the caprylic-capric acid.
3. The cake according to claim 2, wherein the concentration of ethylene glycol in the high concentration ethylene glycol raffinate in step (1) is 90%.
4. The high-concentration ammonia color removal cake as claimed in claim 2, wherein in the step (2), the reflux reaction time is 5-6h, and stirring is carried out during the reflux reaction at a stirring speed of 80-90 r/min.
5. The high-strength ammonia-removing color cake as claimed in claim 1, wherein: the coupling agent is a monoalkoxy pyrophosphate titanate coupling agent.
6. The high-strength ammonia-removing color cake as claimed in claim 1, wherein: the toughening agent is ethylene-vinyl acetate copolymer.
7. The method of making a high consistency cake having ammonia removed therefrom according to any of claims 1 to 6, comprising the steps of: (1) plasticizing: the raw materials are put into an internal mixer for plasticizing and melting to obtain a plasticized melt, the temperature is 120-;
(2) grinding: grinding the plasticized melt obtained in the step (1) for 2-3 times by a three-roll grinder, wherein the grinding temperature is 90-100 ℃, each time is 15-20min, and the pressure is 5-10 kg;
(3) molding: tabletting and forming by a three-roller open mill at 40-50 ℃.
8. Use of the high concentration ammonia-removing color cake of any of claims 1-6 for removing ammonia from a PVB foamed product.
9. A method for removing ammonia by using a high-concentration ammonia-removing color cake, wherein the high-concentration ammonia-removing color cake as described in any one of claims 1 to 6 is added to raw materials for preparing a PVB foaming product and is uniformly mixed with the raw materials, and the ratio of the amount of the high-concentration ammonia-removing color cake to the amount of a foaming agent in the raw materials for the PVB foaming product is (0.5-1): 1.
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| CN106633560A (en) * | 2016-12-28 | 2017-05-10 | 李勇军 | Color masterbatch and manufacturing method |
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