CN111939739A - Low-temperature applicable automobile urea solution and preparation method thereof - Google Patents
Low-temperature applicable automobile urea solution and preparation method thereof Download PDFInfo
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- CN111939739A CN111939739A CN202010855302.2A CN202010855302A CN111939739A CN 111939739 A CN111939739 A CN 111939739A CN 202010855302 A CN202010855302 A CN 202010855302A CN 111939739 A CN111939739 A CN 111939739A
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D53/34—Chemical or biological purification of waste gases
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- F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
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- F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
- F01N3/08—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous
- F01N3/10—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust
- F01N3/18—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust characterised by methods of operation; Control
- F01N3/20—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust characterised by methods of operation; Control specially adapted for catalytic conversion ; Methods of operation or control of catalytic converters
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- F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
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Abstract
The invention discloses a low-temperature applicable automobile urea solution and a preparation method thereof, wherein the urea solution comprises four components of ultrapure water, urea, 1, 4-butyrolactone and ethanol, and the preparation method comprises the steps of taking the ultrapure water as a dispersion medium, adding urea particles, fully dissolving, adding the 1, 4-butyrolactone and the ethanol for compounding, and fully mixing to obtain the urea solution. The reaction process used in the invention is simple and convenient, green and environment-friendly, and has high repeatability. The vehicle urea solution provided by the invention has a simple formula, is easy to operate, and is suitable for large-scale production. In the formula, the ethanol and the 1, 4-butyrolactone are common chemical substances, are green and environment-friendly, and do not contain S, P and other environmentally harmful substances. According to the low-temperature applicable automobile urea solution and the preparation method thereof disclosed by the invention, metal ions and chloride ions are not introduced, so that the detection amount of carbonate and chloride cannot exceed the standard, and the freezing point of the urea solution can be adjusted by adjusting the proportion of each component in the formula.
Description
Technical Field
The invention relates to the technical field of diesel engine tail gas treatment, in particular to a low-temperature applicable automobile urea solution and a preparation method thereof.
Background
With the increasing amount of automobiles, particularly diesel vehicles, in China, the emission of nitrogen oxides and nitrogen oxidesThe harm of particulate matter to human health and the atmospheric environment has raised great concern. The pollution caused by diesel trucks is even more serious, and the main pollutant emission of diesel engines is NOX(Nitrogen oxides) and PM (solid particulate matter), the emission of PM can be effectively controlled by fully combusting diesel oil in an engine by technical means, but NOXThe emission control is to reduce the emission to N in the exhaust process2(Nitrogen) and H2And O (water), wherein the necessary reducing agent in the process is automobile urea liquid, tail gas enters an exhaust pipe from a turbocharger, a urea metering injection device is arranged on the exhaust pipe, and the urea liquid is injected when the temperature reaches 300-500 ℃ to reduce the reaction into nitrogen and water, so that the pollution to the environment is avoided.
For example, chinese patent CN 107138044B discloses a low-temperature urea solution for diesel vehicles and a preparation method thereof, which uses four components including high-purity water, urea, small-molecular liquid alcohol-amine substances and small-molecular liquid alcohol substances to mix to prepare the low-temperature urea solution for vehicles, but the alcohol-amine substances are weakly alkaline substances and corrode parts in the vehicles after long-term use. For example, Chinese patent CN 102213126B, CN 102213124B, an ultra-low temperature urea solution composition for vehicles, CN 104675483A, a low freezing point nitrogen oxide reducing agent and a preparation method thereof, and CN 104533577A, an ultra-low freezing point nitrogen oxide and a preparation method thereof, adopt small molecular liquid alcohols as composite additives, but the components are relatively complex, the process difficulty is increased, in addition, the compositions or the methods contain formamide which is flammable, and can decompose virulent hydrogen cyanide in the presence of a catalyst, and the composition or the method can strongly corrode brass, lead and rubber, so that the storage and the transportation are inconvenient. Therefore, there is a need for an improved process for preparing urea solution for vehicles to solve the above problems, and satisfy the needs of industrial production and practical use.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a low-temperature applicable automobile urea solution and a preparation method thereof. By adding the 1, 4-butyrolactone and the ethanol, the preparation method is simplified, and the freezing point of the prepared automobile urea solution can be controlled by the proportion of the additive.
In order to achieve the purpose, the invention adopts the following technical scheme:
the low-temperature applicable automobile urea solution consists of the following components: ultrapure water, urea, 1, 4-butyrolactone and absolute ethyl alcohol, wherein the mass ratio of the components is as follows: ultrapure water: urea: 1, 4-butyrolactone: ethanol is 50-80:20-35:5-40: 1-20.
A preparation method of low-temperature applicable automobile urea solution comprises the following steps:
s1, adding urea into ultrapure water serving as a medium, and fully stirring for 10-120 minutes to obtain a clear and transparent mixed solution;
s2, adding 1, 4-butyrolactone and ethanol into the mixed solution obtained in the step S1 under the stirring condition, and stirring for 30-120 minutes to obtain clear and transparent low-temperature applicable automobile urea solution.
In the mixed solution of the step S1, the mass portion of urea in the mixed solution is 20 to 35 parts, preferably 31 to 33 parts.
The stirring method in the step S1 is bubbling stirring, and the pressure of bubbling is 1.1X 105Pa-1.5×105Pa, preferably a bubbling pressure of 1.30X 105Pa-1.35×105Pa。
In the low-temperature applicable automobile urea solution obtained in the step S2, the mass portion of the 1, 4-butyrolactone is 5-40 parts, preferably 10-30 parts.
In the low-temperature applicable automobile urea solution obtained in step S2, the mass portion of ethanol is 1 to 20 parts, preferably 2 to 10 parts.
The stirring method in the step S2 is bubbling stirring, and the pressure of bubbling is 1.1X 105Pa-1.5×105Pa, preferably a bubbling pressure of 1.30X 105Pa-1.35×105Pa。
The invention takes ultrapure water as a dispersion medium, adds urea particles, adds 1, 4-butyrolactone and ethanol after full dissolution for compounding, and obtains the urea solution which can be applied in a low-temperature environment (minus 25 ℃) after full mixing. All reaction processes are simple and convenient, green and environment-friendly, and high in repeatability.
The 1, 4-butyrolactone and absolute ethyl alcohol used in the invention are analytically pure.
1, 4-butyrolactone is also known as gamma-butyrolactone, 4-hydroxybutyrolactone. Is a colorless oily liquid, can be mixed with water, and is dissolved in methanol, ethanol, acetone, diethyl ether and benzene. The data show that 1, 4-butyrolactone has a freezing point of about-43.53 deg.C and a boiling point of 204 deg.C, and is a non-electrolyte solution that is less volatile. Experiments prove that the freezing point depression rule of the non-electrolyte dilute solution difficult to volatilize also follows Raoult's law, namely the freezing point depression value is in direct proportion to the molarity of the solution. The invention shows that the freezing point of the solution is obviously reduced after a certain amount of 1, 4-butyrolactone is added into the urea.
Ethanol is a colorless clear liquid, free flowing, with a freezing point of-114.1 ℃. It is easy to absorb water from air, and can be mutually dissolved with water, chloroform, ethyl ether and other organic solvents in any proportion. Because the Henry coefficient of ethanol is larger, the freezing point of the urea solution can be reduced and the fluidity of the urea solution can be increased by adding a proper amount of ethanol. From the principle analysis that the principles applied to the reduction of the freezing point of urea by 1, 4-butyrolactone and absolute ethyl alcohol are different, we speculate that 1, 4-butyrolactone and absolute ethyl alcohol have a superimposed effect on the reduction of the freezing point of urea solution. Research shows that small molecular alcohols such as methanol, ethanol, propanol, isopropanol and the like can reduce the freezing point of the urea solution. For the reasons of environmental protection, cost, safety and the like, the invention selects ethanol and other homologues of ethanol, such as methanol, propanol, isopropanol and other micromolecular alcohols, as protection contents.
In addition, the technical advantages of the invention are also embodied in that:
the vehicle urea solution provided by the invention has a simple formula, is easy to operate, and is suitable for large-scale production. In the formula, the ethanol and the 1, 4-butyrolactone are common chemical substances, are green and environment-friendly, and do not contain S, P and other environmentally harmful substances. According to the low-temperature applicable automobile urea solution and the preparation method thereof, metal ions and chloride ions are not introduced, so that the detected amounts of carbonate and chloride cannot exceed the standard, and the freezing point of the urea solution can be adjusted by adjusting the proportion of each component in the formula.
Detailed Description
The present invention will be further described with reference to the following examples.
In the present specification, the terms "upper", "lower", "left", "right", "middle" and "one" are used for clarity of description only, and are not used to limit the scope of the present invention, and changes or modifications of the relative relationship between the terms and the terms are also considered to be within the scope of the present invention without substantial technical changes.
The instruments, reagents, materials and the like used in the following examples are conventional instruments, reagents, materials and the like in the prior art and are commercially available in a normal manner unless otherwise specified. Unless otherwise specified, the experimental methods, detection methods, and the like described in the following examples are conventional experimental methods, detection methods, and the like in the prior art.
Example 1:
the low-temperature applicable automobile urea solution comprises the following components: ultrapure water, urea, 1, 4-butyrolactone and ethanol. The preparation method comprises the following steps:
s1, adding 28g of urea particles into 60g of ultrapure water, introducing air, bubbling, and stirring until the urea is completely dissolved, wherein the bubbling pressure is 1.3 multiplied by 105Pa。
S2, under the bubbling pressure of 1.3 multiplied by 105And (4) under Pa, adding 10g of 1, 4-butyrolactone and 2g of absolute ethyl alcohol into the mixed solution obtained in the step S1, and carrying out bubbling stirring for 30min to obtain the low-temperature applicable automobile urea solution.
And (3) placing a proper amount of prepared automobile urea solution into a freezing point test tube, and inserting a thermometer which is calibrated by metering into a proper position in the test tube. And inserting the test tube filled with the automobile urea solution and the thermometer into a freezing point tester. After start-up, the freezing temperature is recorded when a large amount of crystallization has occurred.
According to experimental results, the freezing point of the low-temperature applicable automobile urea solution obtained in the embodiment is-16 ℃.
Example 2:
the low-temperature applicable automobile urea solution comprises the following components: ultrapure water, urea, 1, 4-butyrolactone and ethanol. The preparation method comprises the following steps:
s1, adding 30g of urea particles into 58g of ultrapure water, introducing air, bubbling, and stirring until the urea is completely dissolved, wherein the bubbling pressure is 1.2 multiplied by 105Pa。
S2. under the bubbling pressure of 1.2X 105And (4) under Pa, adding 9g of 1, 4-butyrolactone and 3g of absolute ethyl alcohol into the mixed solution obtained in the step S1, and carrying out bubbling stirring for 40min to obtain the low-temperature applicable automobile urea solution.
And (3) placing a proper amount of prepared automobile urea solution into a freezing point test tube, and inserting a thermometer which is calibrated by metering into a proper position in the test tube. And inserting the test tube filled with the automobile urea solution and the thermometer into a freezing point tester. After start-up, the freezing temperature is recorded when a large amount of crystallization has occurred.
According to experimental results, the freezing point of the low-temperature applicable automobile urea solution obtained in the embodiment is-18 ℃.
Example 3:
the low-temperature applicable automobile urea solution comprises the following components: ultrapure water, urea, 1, 4-butyrolactone and ethanol. The preparation method comprises the following steps:
s1, adding 31g of urea particles into 55g of ultrapure water, introducing air, bubbling, and stirring until the urea is completely dissolved, wherein the bubbling pressure is 1.3 multiplied by 105Pa。
S2, under the bubbling pressure of 1.3 multiplied by 105And (4) adding 12g of 1, 4-butyrolactone and 2g of absolute ethyl alcohol into the mixed solution obtained in the step S1 under Pa, and carrying out bubbling stirring for 20min to obtain the low-temperature applicable automobile urea solution.
And (3) placing a proper amount of prepared automobile urea solution into a freezing point test tube, and inserting a thermometer which is calibrated by metering into a proper position in the test tube. And inserting the test tube filled with the automobile urea solution and the thermometer into a freezing point tester. After start-up, the freezing temperature is determined when a large amount of crystallization has occurred.
According to experimental results, the freezing point of the low-temperature applicable automobile urea solution obtained in the embodiment is-20 ℃.
Example 4:
the low-temperature applicable automobile urea solution comprises the following components: ultrapure water, urea, 1, 4-butyrolactone and ethanol. The preparation method comprises the following steps:
s1, taking 52g of ultrapure water, adding 30g of urea particles, introducing air, bubbling, and stirring until the urea is completely dissolved, wherein the bubbling pressure is 1.2 multiplied by 105Pa。
S2, under the bubbling pressure of 1.3 multiplied by 105And (4) under Pa, adding 14g of 1, 4-butyrolactone and 4g of absolute ethyl alcohol into the mixed solution obtained in the step S1, and carrying out bubbling stirring for 40min to obtain the low-temperature applicable automobile urea solution.
And (3) placing a proper amount of prepared automobile urea solution into a freezing point test tube, and inserting a thermometer which is calibrated by metering into a proper position in the test tube. And inserting the test tube filled with the automobile urea solution and the thermometer into a freezing point tester. After start-up, the freezing temperature is recorded when a large amount of crystallization has occurred.
According to experimental results, the freezing point of the low-temperature applicable automobile urea solution obtained in the embodiment is-22 ℃.
Example 5:
the low-temperature applicable automobile urea solution comprises the following components: ultrapure water, urea, 1, 4-butyrolactone and ethanol. The preparation method comprises the following steps:
s1, taking 51g of ultrapure water, adding 29g of urea particles, introducing air, bubbling, and stirring until the urea is completely dissolved, wherein the bubbling pressure is 1.35 multiplied by 105Pa。
S2, under the bubbling pressure of 1.35 multiplied by 105And under Pa, adding 16g of 1, 4-butyrolactone and 4g of absolute ethyl alcohol into the mixed solution obtained in the step S1, and carrying out bubbling stirring for 20min to obtain the low-temperature applicable automobile urea solution.
And (3) placing a proper amount of prepared automobile urea solution into a freezing point test tube, and inserting a thermometer which is calibrated by metering into a proper position in the test tube. And inserting the test tube filled with the automobile urea solution and the thermometer into a freezing point tester. After start-up, the freezing temperature is recorded when a large amount of crystallization has occurred.
According to experimental results, the freezing point of the low-temperature applicable automobile urea solution obtained in the embodiment is-23 ℃.
Example 6:
the low-temperature applicable automobile urea solution comprises the following components: ultrapure water, urea, 1, 4-butyrolactone and ethanol. The preparation method comprises the following steps:
s1, adding 28g of urea particles into 55g of ultrapure water, introducing air, bubbling, and stirring until the urea is completely dissolved, wherein the bubbling pressure is 1.45 multiplied by 105Pa。
S2, under the bubbling pressure of 1.45 multiplied by 105Under Pa, adding 16g of 1, 4-butyrolactone and 1g of absolute ethyl alcohol into the mixed solution obtained in the step S1, and carrying out bubbling stirring for 30min to obtain the low-temperature applicable automobile urea solution.
And (3) placing a proper amount of prepared automobile urea solution into a freezing point test tube, and inserting a thermometer which is calibrated by metering into a proper position in the test tube. And inserting the test tube filled with the automobile urea solution and the thermometer into a freezing point tester. After start-up, the freezing temperature is recorded when a large amount of crystallization has occurred.
According to experimental results, the freezing point of the low-temperature applicable automobile urea solution obtained in the embodiment is-22.5 ℃.
Control group 1:
the urea solution for the vehicle comprises the following components: ultrapure water and urea. The preparation method comprises the following steps:
adding 33g of urea particles into 67g of ultrapure water, introducing air, bubbling, stirring until the urea is completely dissolved, wherein the bubbling pressure is 1.4 multiplied by 105Pa, and bubbling and stirring for 30min to obtain the vehicle urea solution.
And (3) placing a proper amount of prepared automobile urea solution into a freezing point test tube, and inserting a thermometer which is calibrated by metering into a proper position in the test tube. And inserting the test tube filled with the automobile urea solution and the thermometer into a freezing point tester. After start-up, the freezing temperature is recorded when a large amount of crystallization has occurred.
The experiment shows that the freezing point of the urea solution for vehicles obtained by the control group is-11.5 ℃.
Control group 2:
the urea solution for the vehicle comprises the following components: ultrapure water, urea and 1, 4-butyrolactone. The preparation method comprises the following steps:
s1, adding 28g of urea particles into 60g of ultrapure water, introducing air, bubbling, and stirring until the urea is completely dissolved, wherein the bubbling pressure is 1.4X 105 Pa.
S2, adding 12g of 1, 4-butyrolactone into the mixed solution obtained in the step S1 under the bubbling pressure of 1.4X 105Pa, and carrying out bubbling stirring for 25min to obtain the automotive urea solution.
And (3) placing a proper amount of prepared automobile urea solution into a freezing point test tube, and inserting a thermometer which is calibrated by metering into a proper position in the test tube. And inserting the test tube filled with the automobile urea solution and the thermometer into a freezing point tester. After start-up, the freezing temperature is recorded when a large amount of crystallization has occurred.
The experiment shows that the freezing point of the urea solution for vehicles obtained by the control group is-18.5 ℃.
Is the freezing point in this control below that of examples 1 and 2, is adjustment required?
Control group 3:
the urea solution for the vehicle comprises the following components: ultrapure water, urea and ethanol. The preparation method comprises the following steps:
s1, taking 65g of ultrapure water, adding 30g of urea particles, introducing air, bubbling, and stirring until the urea is completely dissolved, wherein the bubbling pressure is 1.35X 105 Pa.
S2, adding 5g of absolute ethyl alcohol into the mixed solution obtained in the step S1 under the bubbling pressure of 1.35X 105Pa, and carrying out bubbling stirring for 30min to obtain the vehicle urea solution.
And (3) placing a proper amount of prepared automobile urea solution into a freezing point test tube, and inserting a thermometer which is calibrated by metering into a proper position in the test tube. And inserting the test tube filled with the automobile urea solution and the thermometer into a freezing point tester. After start-up, the freezing temperature is recorded when a large amount of crystallization has occurred.
The experiment shows that the freezing point of the low-temperature applicable automobile urea solution obtained by the control group is-15.5 ℃.
| Numbering | Ultrapure water (g) | Urea (g) | 1, 4-butyrolactone (g) | Ethanol (g) | Freezing point (. degree. C.) |
| Example 1 | 60 | 28 | 10 | 2 | -16 |
| Example 2 | 58 | 30 | 9 | 3 | -18 |
| Example 3 | 55 | 31 | 12 | 2 | -20 |
| Example 4 | 52 | 30 | 14 | 4 | -22 |
| Example 5 | 51 | 29 | 16 | 4 | -23 |
| Example 6 | 55 | 28 | 16 | 1 | -22.5 |
| Control group 1 | 67 | 33 | / | / | -11.5 |
| Control group 2 | 60 | 28 | 12 | / | -18.5 |
| Control group 3 | 65 | 30 | / | 5 | -15.5 |
The comparison of data in the table shows that after the two additives of the 1, 4-butyrolactone and the ethanol are added, the freezing point of the automobile urea solution is obviously reduced compared with the addition of one additive or the other additive, which shows that the method provided by the invention is effective and has a theoretical basis of large-scale popularization.
The freezing point tester used in all the above examples is a DKL-218SH/T0090 type freezing point tester from Kunlun Petroleum instruments, Inc.
Although the present invention has been described with reference to the specific embodiments, it should be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.
Claims (10)
1. The low-temperature applicable automobile urea solution is characterized by comprising the following components: ultrapure water, urea, 1, 4-butyrolactone and ethanol, wherein the components are ultrapure water: urea: 1, 4-butyrolactone: the absolute ethyl alcohol is 50-80:20-35:5-40: 1-20.
2. A preparation method of low-temperature applicable automobile urea solution is characterized by comprising the following steps:
s1, adding urea into ultrapure water serving as a medium, and fully stirring to obtain a mixed solution;
s2, adding 1.4-butyrolactone and ethanol into the mixed solution obtained in the step S1 under the stirring condition to obtain the low-temperature applicable automobile urea solution.
3. The method for preparing the urea solution for the low-temperature suitable vehicle as claimed in claim 1, wherein the urea is 20-35 parts by weight.
4. The method for preparing the urea solution for the low-temperature suitable vehicle as claimed in claim 1, wherein the mass fraction of the urea is 31-33 parts.
5. The method for preparing low-temperature urea solution suitable for vehicles according to claim 1, wherein the 1, 4-butyrolactone is present in an amount of 5-40 parts by weight.
6. The method for preparing low-temperature urea solution suitable for vehicles according to claim 1, wherein the 1, 4-butyrolactone is present in an amount of 10-30 parts by weight.
7. The method for preparing the urea solution for the low-temperature suitable vehicle as claimed in claim 1, wherein the ethanol is 1-20 parts by weight.
8. The method for preparing the urea solution for the low-temperature suitable vehicle as claimed in claim 1, wherein the ethanol is used in an amount of 2 to 10 parts by weight.
9. The method for preparing urea solution for vehicles at low temperature according to claim 2, wherein the agitation in steps S1 and S2 is bubbling agitation with a bubbling pressure of 1.1X 105Pa-1.5×105Pa, the bubbling time is 10min-200 min.
10. The method for preparing urea solution for vehicles at low temperature according to claim 2, wherein the stirring method in steps S1 and S2 is bubbling stirring, and the bubbling pressure is 1.30X 105Pa-1.35×105Pa, the bubbling time is 30-60 min.
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| CN112370968A (en) * | 2020-12-03 | 2021-02-19 | 山东欧蓝素汽车环保科技有限公司 | Novel vehicle urea solution and preparation method thereof |
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