Summary of the invention
Goal of the invention of the present invention is: for the problem of above-mentioned existence, a kind of ammonium chloride fluid loss agent and preparation method thereof is provided, after ammonium chloride fluid loss agent of the present invention joins in ammonium chloride, can enlarge markedly the filtration efficiency of whizzer, reduce the moisture content in ammonium chloride product, improve the production capacity of drying unit, reduce the energy consumption of oven dry link, shorten time of drying, therefore, the present invention has economic benefit preferably.
The technical solution used in the present invention is as follows:
A kind of ammonium chloride fluid loss agent is comprised of the component of following mass percent:
Mass percent is the dodecyl iso-octyl maleic acid diester sodium sulfonate aqueous solution 40~70% of 50%wt;
Mass percent is the Dodecyl trimethyl ammonium chloride aqueous solution 5~15% of 70%wt;
Isooctyl alcohol 5~10%;
Water surplus.
As preferably, above-mentioned ammonium chloride fluid loss agent is comprised of the component of following mass percent:
Mass percent is the dodecyl iso-octyl maleic acid diester sodium sulfonate aqueous solution 50~60% of 50%wt;
Mass percent is the Dodecyl trimethyl ammonium chloride aqueous solution 7~10% of 70%wt;
Isooctyl alcohol 6~8%;
Water surplus.
Wherein, the molecular structural formula of dodecyl iso-octyl maleic acid diester sodium sulfonate is as follows:
The described dodecyl iso-octyl maleic acid diester sodium sulfonate aqueous solution is prepared by following methods:
Isooctyl alcohol, lauryl alcohol, maleic anhydride are joined in reactor by the mol ratio of 1:1:1-1.05, the tosic acid that adds wherein again isooctyl alcohol and lauryl alcohol total mass 1.0%, 110 ℃-130 ℃ reactions 3-4 hour, then be cooled to room temperature, use again 5%(wt) aqueous sodium carbonate washing, after removing water layer, then add wherein sodium sulfite solution, 90 ℃ of reactions 1.5 hours, namely get product;
The mol ratio of described maleic anhydride and sodium bisulfite is 1:1.1-1.3.
In the dodecyl iso-octyl maleic acid diester sodium sulfonate aqueous solution that is obtained by aforesaid method, the quality percentage composition of dodecyl iso-octyl maleic acid diester sodium sulfonate 〉=50%.
Wherein, the reaction equation of preparation dodecyl iso-octyl maleic acid diester sodium sulfonate is as follows:
Be used for the preparation method of described ammonium chloride fluid loss agent, comprise the steps:
The Dodecyl trimethyl ammonium chloride aqueous solution, isooctyl alcohol, water are joined in reactor by proportioning stir, add the dodecyl iso-octyl maleic acid diester sodium sulfonate aqueous solution in whipping process, mixing gets final product.
During use, use this ammonium chloride of 0.2~0.5 ㎏ with the ratio of precipitation agent in producing 1 ton of finished product ammonium chloride, add ammonium chloride fluid loss agent in ammonium chloride, then the mixture that obtains is carried out centrifuging and get final product.
Dodecyl iso-octyl maleic acid diester sodium sulfonate in the present invention and Dodecyl trimethyl ammonium chloride adopt the form of the aqueous solution, are convenient in process of production, and raw material is mixed.
In ammonium chloride when adding ammonium chloride fluid loss agent of the present invention to the whizzer filtration, bioactive molecule in ammonium chloride fluid loss agent can uniform spreading to the ammonium chloride particle surface, asymmetric hydrophobic group wherein outwards stretches, thereby destroy the hydration shell on ammonium chloride particle surface, thereby greatly reduce the multilayer absorption of bioactive molecule, improve the perviousness of water in ammonium chloride, accelerate the filtration speed of water, increase the filtration efficiency of whizzer, reduce the moisture content in ammonium chloride product.The contriver finds through great many of experiments, a small amount of this ammonium chloride fluid loss agent of centrifuge treating interpolation that filters at ammonium chloride can improve filtration speed, reduce the water content of ammonium chloride product, because ammonium chloride can not be taked high temperature drying, otherwise the loss meeting of ammonium chloride increases greatly, and therefore, the method has reduced the energy consumption of rear end drying, improve the production capacity of drying efficiency oven dry and device, reduced the energy consumption of oven dry link.
Ammonium chloride fluid loss agent of the present invention can significantly improve the ammonium chloride filtering rate, reduces the ammonium chloride moisture content, reduces time of drying, enhances productivity, and has higher economic benefit.
Embodiment
Disclosed all features in this specification sheets, or the step in disclosed all methods or process except mutually exclusive feature and/or step, all can make up by any way.
Disclosed arbitrary feature in this specification sheets (comprising any accessory claim, summary and accompanying drawing) is unless special narration all can be replaced by other equivalences or the alternative features with similar purpose.That is, unless special narration, each feature is an example in a series of equivalences or similar characteristics.
The dodecyl iso-octyl maleic acid diester sodium sulfonate that uses in embodiment in the present invention prepares by the following method:
103 kilograms of 130.2 kilograms of isooctyl alcohol, 186.4 kilograms of lauryl alcohols, maleic anhydride are joined in reactor, add wherein again 3.2 kilograms of tosic acid, 110 ℃-130 ℃ reactions 3-4 hour, then be cooled to room temperature, with the washing of 5% aqueous sodium carbonate, after removing water layer, then add wherein 655.8 kilograms of sodium bisulfite 20% aqueous solution again, 90 ℃ of reactions 1.5 hours, obtain the dodecyl iso-octyl maleic acid diester sodium sulfonate aqueous solution.In the dodecyl iso-octyl maleic acid diester sodium sulfonate aqueous solution, the quality percentage composition of dodecyl iso-octyl maleic acid diester sodium sulfonate 〉=50%.
Wherein, the reaction equation of preparation dodecyl iso-octyl maleic acid diester sodium sulfonate is as follows:
Wherein, the isooctyl alcohol of use, lauryl alcohol, maleic anhydride, tosic acid manufacturer be respectively: prosperous sharp source, Guangdong company, the auspicious auspicious chemical company in Zibo, Shanghai Sheng Lei chemical company, Shandong Yunxiang chemical company.
In all embodiment of the present invention, adopt following measurement of test method ammonium chloride fluid loss agent to reduce the effect of product moisture:
Claim 100g to take from ammonium chloride on whizzer in beaker, after adding the 200ml ammonium chloride mother liquor, then add the ammonium chloride fluid loss agent of metering, be made into ammonium chloride suspension, open water-ring vacuum pump, Büchner funnel with Φ 100 carries out suction filtration 30s to ammonium chloride suspension, uses the dry also weighing bottle of constant weight under 100-105 ℃ in advance, takes the 5g sample, be accurate to 0.001g, be placed in 100^-105 ℃ of loft drier, be dried to constant weight (being no more than 4h), the weightless water ratio of measuring filter cake of weighing.
In the present invention, the preparation method of ammonium chloride fluid loss agent is as follows:
Press each component of proportion speed weighing, and join in reactor with whipping appts, stir it is fully mixed, namely get product.
Embodiment 1 and comparative example 1-4
Table 1 has provided respectively the portion rate of each component in embodiment 1 and comparative example 1-4.Wherein, A component in embodiment 1 and comparative example 1-4 is respectively: mass percent is the dodecyl iso-octyl maleic acid diester sodium sulfonate aqueous solution (the present invention's self-control), Sodium dodecylbenzene sulfonate (buying in Jinan Zhong Ze chemical company), isooctyl alcohol sodium sulfosuccinic diester, polyoxyethylene nonylphenol ether (buying the permanent chemical company that wins in the Guangzhou), the Nekal BX (buying in perseverance Tonghua, Shangyu city work company) of 50%wt, and the B component is the Dodecyl trimethyl ammonium chloride aqueous solution that mass percent is 70%wt.
The ratio of component of table 1 embodiment 1 and comparative example 1-4
? |
Embodiment 1 |
The comparative example 1 |
The comparative example 2 |
The comparative example 3 |
The comparative example 4 |
The A component |
50 |
50 |
50 |
50 |
50 |
The B component |
7 |
7 |
7 |
7 |
7 |
Isooctyl alcohol |
8 |
8 |
8 |
8 |
8 |
Water |
35 |
35 |
35 |
35 |
35 |
The production technique of comparative example 1-4 and embodiment 1 is identical.
Add the precipitation agent in ammonium chloride: respectively with embodiment 1 and the prepared product of comparative example 1-4, the ratio of adding 0.3 ㎏ precipitation agent according to ammonium chloride per ton joins in ammonium chloride, and rear filtration stirs.Ammonium chloride does not wherein add any auxiliary agent from Production of Ammonium Chloride enterprise.
According to foregoing test method, respectively the ammonium chloride (blank example) that does not add ammonium chloride fluid loss agent, the ammonium chloride (embodiment 1, comparative example 1-4) that has added embodiment 1 and comparative example 1-4 product are analyzed, calculate its moisture reduced rate, corresponding test result is as shown in table 2.
The test result of table 2 embodiment 1 and comparative example 1-4
? |
Blank example |
Embodiment 1 |
The comparative example 1 |
The comparative example 2 |
The comparative example 3 |
The comparative example 4 |
Moisture (%) |
7.5 |
5.4 |
6.7 |
6.3 |
7.2 |
6.9 |
As can be seen from Table 2, compare with the blank example of not adding ammonium chloride fluid loss agent, after having added active substance, in ammonium chloride, moisture content all decreases, but embodiment 1 obviously is better than comparative example 1-4.
Embodiment 2 and comparative example 5-8
Table 3 has provided respectively the portion rate of each component in embodiment 2 and comparative example 5-8.Wherein, A component in embodiment 2 and comparative example 5-8 is respectively: mass percent is the dodecyl iso-octyl maleic acid diester sodium sulfonate aqueous solution (the present invention's self-control), sodium lauryl sulphate (buy in Guangzhou prosperous platinum trading company), oleylamide trimethyl-glycine (buy in Nanjing safe climing knob chemical industry company limited), polyoxyethylene nonylphenol ether (buying in Hai'an, Jiangsu petroleum chemical plant), the isooctyl alcohol sodium sulfosuccinic diester (self-control) of 50%wt, and the B component is the Dodecyl trimethyl ammonium chloride aqueous solution that mass percent is 70%wt.
The ratio of component of table 3 embodiment 2 and comparative example 5-8
? |
Embodiment 2 |
The comparative example 5 |
The comparative example 6 |
The comparative example 7 |
The comparative example 8 |
The A component |
55 |
55 |
55 |
55 |
55 |
The B component |
10 |
10 |
10 |
10 |
10 |
Isooctyl alcohol |
6 |
6 |
6 |
6 |
6 |
Water |
29 |
29 |
29 |
29 |
29 |
The production technique of comparative example 5-8 and embodiment 2 is identical.
Add the precipitation agent in ammonium chloride: respectively with embodiment 2 and the prepared product of comparative example 5-8, the ratio of adding 0.3 ㎏ precipitation agent according to ammonium chloride per ton joins in ammonium chloride, and rear filtration stirs.Ammonium chloride does not wherein add any auxiliary agent from Production of Ammonium Chloride enterprise.
According to foregoing test method, respectively the ammonium chloride (blank example) that does not add ammonium chloride fluid loss agent, the ammonium chloride (embodiment 2, comparative example 5-8) that has added embodiment 2 and comparative example 5-8 product are analyzed, calculate its moisture reduced rate, corresponding test result is as shown in table 4.
The test result of table 4 embodiment 2 and comparative example 5-8
? |
Blank example |
Embodiment 2 |
The comparative example 5 |
The comparative example 6 |
The comparative example 7 |
The comparative example 8 |
Moisture (%) |
7.8 |
4.6 |
6.3 |
7.1 |
7.4 |
6.3 |
As can be seen from Table 4, compare with the blank example of not adding ammonium chloride fluid loss agent, after having added active substance, in ammonium chloride, moisture content all decreases, but embodiment 2 effects are the most obvious, and its moisture reduced rate is 41%.
Embodiment 3 and comparative example 9-12
Table 5 has provided respectively the portion rate of each component in embodiment 3 and comparative example 9-12.wherein, A component in embodiment 3 and comparative example 9-12 is respectively: mass percent is the dodecyl iso-octyl maleic acid diester sodium sulfonate aqueous solution (the present invention's self-control) of 50%wt, Sodium dodecylbenzene sulfonate (buying in Jinan Zhong Ze chemical company), dispersing agent NNO (buying in Anyang dicyclo auxiliary agent company limited), polyoxyethylene nonylphenol ether (buying the permanent chemical company that wins in Guangzhou), Varisoft 432PPG (Jiangsu Kai Lida chemistry company limited), the B component is the Dodecyl trimethyl ammonium chloride aqueous solution that mass percent is 70%wt.
The ratio of component of table 5 embodiment 3 and comparative example 9-12
? |
Embodiment 3 |
The comparative example 9 |
The comparative example 10 |
The comparative example 11 |
The comparative example 12 |
The A component |
60 |
60 |
60 |
60 |
60 |
The B component |
10 |
10 |
10 |
10 |
10 |
Isooctyl alcohol |
8 |
8 |
8 |
8 |
8 |
Water |
22 |
22 |
22 |
22 |
22 |
The production technique of comparative example 9-12 and embodiment 3 is identical.
Add the precipitation agent in ammonium chloride: respectively with embodiment 3 and the prepared product of comparative example 9-12, the ratio of adding 0.3 ㎏ precipitation agent according to ammonium chloride per ton joins in ammonium chloride, and rear filtration stirs.Ammonium chloride does not wherein add any auxiliary agent from Production of Ammonium Chloride enterprise.
According to foregoing test method, respectively the ammonium chloride (blank example) that does not add ammonium chloride fluid loss agent, the ammonium chloride (embodiment 3, comparative example 9-12) that has added embodiment 3 and comparative example 9-12 product are analyzed, calculate its moisture reduced rate, corresponding test result is as shown in table 4.
The test result of table 6 embodiment 3 and comparative example 9-12
? |
Blank example |
Embodiment 3 |
The comparative example 9 |
The comparative example 10 |
The comparative example 11 |
The comparative example 12 |
Moisture (%) |
6.8 |
3.9 |
5.9 |
5.8 |
6.2 |
5.5 |
As can be seen from Table 6, further increase the actives consumption, comparative example's dewatering effect does not have considerable change, and the dewatering effect of embodiment 3 further improves.Compare with blank example, embodiment 3 reaches 42.6% for the reduced rate of moisture in ammonium chloride.
Embodiment 4 and comparative example 13-16
Table 7 has provided respectively the portion rate of each component in embodiment 4 and comparative example 13-16.Wherein, A component in embodiment 4 and comparative example 13-16 is respectively: mass percent is the dodecyl iso-octyl maleic acid diester sodium sulfonate aqueous solution (the present invention's self-control), alcohol ether phosphate monoester ethanolamine salt (buying in Hai'an, Jiangsu petroleum chemical plant), dimethyl dodecyl amine oxide (Shanghai Jingwei Chemical Co., Ltd.), polyoxyethylene nonylphenol ether (buying the permanent chemical company that wins in Guangzhou), the leveler 102 (Jiangsu Hai'an Petrochemical Plant) of 50%wt, and the B component is the Dodecyl trimethyl ammonium chloride aqueous solution that mass percent is 70%wt.
The ratio of component of table 7 embodiment 4 and comparative example 13-16
? |
Embodiment 4 |
The comparative example 13 |
The comparative example 14 |
The comparative example 15 |
The comparative example 16 |
The A component |
40 |
40 |
40 |
40 |
40 |
The B component |
15 |
15 |
15 |
15 |
15 |
Isooctyl alcohol |
5 |
5 |
5 |
5 |
5 |
Water |
40 |
40 |
40 |
40 |
40 |
The production technique of comparative example 13-16 and embodiment 4 is identical.
Add the precipitation agent in ammonium chloride: respectively with embodiment 4 and the prepared product of comparative example 13-16, the ratio of adding 0.3 ㎏ precipitation agent according to ammonium chloride per ton joins in ammonium chloride, and rear filtration stirs.Ammonium chloride does not wherein add any auxiliary agent from Production of Ammonium Chloride enterprise.
According to foregoing test method, respectively the ammonium chloride (blank example) that does not add ammonium chloride fluid loss agent, the ammonium chloride (embodiment 4, comparative example 13-16) that has added embodiment 4 and comparative example 13-16 product are analyzed, calculate its moisture reduced rate, corresponding test result is as shown in table 4.
The test result of table 8 embodiment 4 and comparative example 13-16
? |
Blank example |
Embodiment 4 |
The comparative example 13 |
The comparative example 14 |
The comparative example 15 |
The comparative example 16 |
Moisture (%) |
7.9 |
5.2 |
6.7 |
6.9 |
5.8 |
6.5 |
As can be seen from Table 8, the successful of embodiment 4 is better than comparative example 13-16.Compare with blank example, embodiment 4 reaches 34.1% for the reduced rate of moisture in ammonium chloride.
Embodiment 5 and comparative example 17-20
Table 9 has provided respectively the portion rate of each component in embodiment 5 and comparative example 17-20.Wherein, A component in embodiment 5 and comparative example 17-20 is respectively: mass percent is the dodecyl iso-octyl maleic acid diester sodium sulfonate aqueous solution (the present invention's self-control), alcohol ether phosphate monoester ethanolamine salt (buying in Hai'an, Jiangsu petroleum chemical plant), dimethyl dodecyl amine oxide (Shanghai Jingwei Chemical Co., Ltd.), polyoxyethylene nonylphenol ether (buying the permanent chemical company that wins in Guangzhou), the leveler 102 (Jiangsu Hai'an Petrochemical Plant) of 50%wt, and the B component is the Dodecyl trimethyl ammonium chloride aqueous solution that mass percent is 70%wt.
The ratio of component of table 9 embodiment 5 and comparative example 17-20
? |
Embodiment 5 |
The comparative example 17 |
The comparative example 18 |
The comparative example 19 |
The comparative example 20 |
The A component |
70 |
70 |
70 |
70 |
70 |
The B component |
5 |
5 |
5 |
5 |
5 |
Isooctyl alcohol |
10 |
10 |
10 |
10 |
10 |
Water |
15 |
15 |
15 |
15 |
15 |
The production technique of comparative example 17-20 and embodiment 5 is identical.
Add the precipitation agent in ammonium chloride: respectively with embodiment 5 and the prepared product of comparative example 17-20, the ratio of adding 0.3 ㎏ precipitation agent according to ammonium chloride per ton joins in ammonium chloride, and rear filtration stirs.Ammonium chloride does not wherein add any auxiliary agent from Production of Ammonium Chloride enterprise.
According to foregoing test method, respectively the ammonium chloride (blank example) that does not add ammonium chloride fluid loss agent, the ammonium chloride (embodiment 5, comparative example 17-20) that has added embodiment 5 and comparative example 17-20 product are analyzed, calculate its moisture reduced rate, corresponding test result is as shown in table 10.
The test result of table 10 embodiment 5 and comparative example 17-20
? |
Blank example |
Embodiment 5 |
The comparative example 17 |
The comparative example 18 |
The comparative example 19 |
The comparative example 20 |
Moisture (%) |
8.0 |
5.0 |
6.6 |
6.4 |
7.3 |
7.0 |
As can be seen from Table 10, further increase the actives consumption, comparative example's dewatering effect does not have considerable change, and the dewatering effect of embodiment 5 increases.Compare with blank example, embodiment 5 reaches 37.5% for the reduced rate of moisture in ammonium chloride.
Prove by simultaneous test, precipitation agent of the present invention can significantly reduce the moisture in ammonium chloride, has significant economic worth.
The present invention is not limited to aforesaid embodiment.The present invention expands to any new feature or any new combination that discloses in this manual, and the arbitrary new method that discloses or step or any new combination of process.