CN103616379B - The quantitative determination method of 4-propyl bromide content in zeolite synthesis waste liquid - Google Patents
The quantitative determination method of 4-propyl bromide content in zeolite synthesis waste liquid Download PDFInfo
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Abstract
The invention discloses the quantitative determination method of 4-propyl bromide content in zeolite synthesis waste liquid, draw the linearity curve (B of the linearity curve A of pure 4-propyl bromide volumetric molar concentration, the waste liquid 4-propyl bromide volumetric molar concentration under different dilution ratio
1..., B
n), by by (B
1..., B
n) linear regression, obtain being no more than with A slope error ± the linearity curve C of 0.02% is the linearity curve of 4-propyl bromide volumetric molar concentration in quantitative determination waste liquid, thus calculates 4-propyl bromide content in waste liquid.Advantage of the present invention is: by setting up the linearity curve A of pure 4-propyl bromide volumetric molar concentration, by adding the 4-propyl bromide of known quantity to waste liquid to be measured, then recurrence correction is carried out to its test result, thus to eliminate in waste liquid impurity to the impact of titration effect, obtain the exact level of 4-propyl bromide in waste liquid, analysis precision can reach more than 95%, and repeatability is high, realize 4-propyl bromide content in quantitative determination waste liquid, thus waste liquid is reused.
Description
Technical field
The present invention relates to the assay method of 4-propyl bromide content in a kind of zeolite synthesis waste liquid.
Background technology
ZSM-5 zeolite is widely used in each fields such as chemical reaction, gas processing and absorption, and be except y-type zeolite, type A zeolite, most widely used zeolitic material in chemical industry, at present, domestic productive capacity reaches ton up to ten thousand.
The synthesis of ZSM-5 zeolite, need using organic quaternary ammonium salts material as organic formwork agent, wherein 4-propyl bromide is the most widely used organic formwork agent.4-propyl bromide is the important cationic surfactant of a class, good with the surfactant compatibility of other type, and there is good emulsification, wetting, solubilising, washing, sterilization, softness, help dye, fixation, a series of performance such as antistatic, its chemical formula is C
12h
28brN.
Because ZSM-5 zeolite takes hydrothermal synthesis method to produce, by being the 4-propyl bromide of 1 ~ 8% containing mass ratio in its waste liquid, COD in waste liquid, ammonia nitrogen and content of halogen is caused to exceed standard.The various physical and chemical indexes in waste liquid are reduced by methods such as traditional oxidation, qi exhaustions, with high costs.In addition, 4-propyl bromide is expensive, is discharged by waste liquid, also can cause unnecessary waste.Therefore, the 4-propyl bromide in recycling waste liquid is from environmental protection or reducing costs aspect is all necessary work.
In order to reach the object of Recycling of waste liquid, first just need the content of the 4-propyl bromide determined in waste liquid.The analytical approach of dimethyl level benzyl ammonium chloride is defined in industry standard HG/T2230-2006 " water treatment agent dimethyl level benzyl ammonium chloride ", namely quaternary ammonium salt and dichlorofluorescein is utilized to generate chelate, when with tetraphenylboron sodium titration, tetraphenylboron sodium displaces dichlorofluorescein and generates with it handsome red mixture from quaternary ammonium salt and dichlorofluorescein, after reaching home, solution changes yellow into by bright red look, then measures the massfraction of quaternary ammonium salt.Other assay method has ion exchange process, the precipitation method, block system etc., but these methods are all the mensuration for long chain quaternary, for 4-propyl bromide, because its main chain is shorter, and ammonium ion easily dissociates, the conclusion error using these assay methods to obtain is very large.
Wu Wen frame etc. has carried out analysis linguistic term to HG/T2230-2006 standard, they utilize tetraphenylboron sodium to react with quaternary ammonium salt in alkaline medium and form white precipitate, use excessive tetraphenylboron sodium by quaternary salt deposit, and excessive tetraphenylboron sodium re-uses cetyl trimethyl ammonium bromide titration, until during terminal, cetyl trimethyl ammonium bromide and titan yellow form pink and show.This solves the difficult problem that the colour developing of low carbon chain quaternary ammonium salt is not obvious, error is larger, measuring accuracy rate to the low carbon chain quaternary ammonium salt solution of massfraction more than 0.1% can reach more than 99.5%.Meanwhile, Li Yan etc., in the method, have studied the impact of concentration of sodium hydroxide solution on precision of analysis, determine the optimal addn of NaOH.
Although HG/T2230-2006 standard such as the job development of Wu Wen frame and Li Yan etc., makes the massfraction of quantitative test tetrapropyl sodium bromide become possibility, in their analytical approach, 4-propyl bromide is all one matter solution, and purity is very high.The waste liquid of ZSM-5 zeolite Hydrothermal Synthesis system, except containing except 4-propyl bromide, also contains a large amount of NaOH, ammoniacal liquor and a large amount of SiO
2the impurity such as granule, the existence of these impurity, when making to use tetraphenylboron sodium back titration, same inevitably existence affects the difficult problems such as titration end-point, thus affects the accuracy of quantitative test.
Summary of the invention
Goal of the invention: for the problems referred to above, the object of this invention is to provide a kind of fast, the method for 4-propyl bromide content in Accurate Determining zeolite synthesis waste liquid.
Technical scheme: the quantitative determination method of 4-propyl bromide content in zeolite synthesis waste liquid, draws the linearity curve (B of the linearity curve A of pure 4-propyl bromide volumetric molar concentration, the waste liquid 4-propyl bromide volumetric molar concentration under different dilution ratio
1..., B
n), by by (B
1..., B
n) linear regression, obtain being no more than with A slope error ± the linearity curve C of 0.02% is the linearity curve of 4-propyl bromide volumetric molar concentration in quantitative determination waste liquid, thus calculates 4-propyl bromide content in waste liquid.
Specifically comprise the following steps:
Step (1) draws the linearity curve A of pure 4-propyl bromide volumetric molar concentration:
A () pipettes the pure 4-propyl bromide solution of 5mL concentration known, with distilled water diluting 50 times; Pipette the tetraphenylboron sodium standard solution of the described pure 4-propyl bromide solution after 5mL dilution, 5mL concentration 0.01mol/L, be placed in conical flask, add 5mL formaldehyde, the NaOH solution of 0.2mL massfraction 20%, the titan yellow indicator solution of 1mL massfraction 0.1% again, be titrated to terminal with the cetyl trimethyl ammonium bromide solution of concentration 0.01mol/L;
B () repeats (a), test the pure 4-propyl bromide solution of multiple different concentration known respectively;
C () is set up coordinate system with the quality of cetyl trimethyl ammonium bromide solution being titrated to terminal and consuming and the volumetric molar concentration of pure 4-propyl bromide solution and is drawn point diagram, obtain linearity curve A and the equation y=4.878 × x-0.0000851271 thereof of pure 4-propyl bromide volumetric molar concentration, wherein the y quality that is the cetyl trimethyl ammonium bromide solution that is titrated to terminal and consumes, x are the volumetric molar concentration of pure 4-propyl bromide;
Step (2) draws the linearity curve (B of 4-propyl bromide volumetric molar concentration in waste liquid
1..., B
n):
D () pipettes 5mL waste liquid, with distilled water diluting 50 times; Pipette described waste liquid, the pure 4-propyl bromide solution of known quality and the tetraphenylboron sodium standard solution of 5mL concentration 0.01mol/L after 5mL dilution, be placed in conical flask, add 5mL formaldehyde, the NaOH solution of 0.2mL massfraction 20%, the titan yellow indicator solution of 1mL massfraction 0.1% again, be titrated to terminal with the cetyl trimethyl ammonium bromide solution of concentration 0.01mol/L;
E () repeats (d), by described waste liquid dilution different multiplying, test respectively;
F () is set up coordinate system with the volumetric molar concentration of 4-propyl bromide in the quality of the cetyl trimethyl ammonium bromide solution being titrated to terminal and consuming and the waste liquid estimated and is drawn point diagram, obtain the linearity curve (B of the 4-propyl bromide volumetric molar concentration of waste liquid under different dilution ratio
1..., B
n);
Step (3) modified line linearity curve (B
1..., B
n): by by (B
1..., B
n) linear regression, obtain being no more than with A slope error ± the linearity curve C of 0.02% is the linearity curve of 4-propyl bromide volumetric molar concentration in quantitative determination waste liquid;
4-propyl bromide content in step (4) quantitative determination zeolite synthesis waste liquid: for certain waste liquid to be measured, according to linearity curve C, by the quality being titrated to the cetyl trimethyl ammonium bromide solution that terminal consumes, 4-propyl bromide content in waste liquid can be obtained.
Contained by described zeolite synthesis waste liquid, component comprises SiO
2solid particle, NaOH, 4 bromide.
Described tetraphenylboron sodium standard solution is prepared by the following method: get aluminium choride 1.0g, is dissolved in 25mL water, and constantly stirring and slowly drip sodium hydroxide solution is 8 ~ 9 to pH value, obtains gel aluminum hydroxide; Get tetraphenylboron sodium 3.5g, the 50mL jolting that adds water makes it to dissolve, and adds described gel aluminum hydroxide 12.5mL, jolts 5 minutes, add sodium chloride 8.3g, fully stir evenly, add water 250mL jolting 15 minutes, leaves standstill 10 minutes, filter with double-deck Medium speed filter paper, dripping sodium hydroxide solution to pH value in filtrate is 8 ~ 9, then is diluted with water to 1000mL and shakes up, and to obtain final product.
Principle of the present invention is: 4-propyl bromide forms white precipitate with sodium tetraphenylborate solution in alkaline medium, uses excessive tetraphenylboron sodium to be precipitated completely by the 4-propyl bromide in waste liquid; Excessive tetraphenylboron sodium and cetyl trimethyl ammonium bromide are formed and precipitate, and use excessive cetyl trimethyl ammonium bromide to be precipitated completely by residual tetraphenylboron sodium; Residual cetyl trimethyl ammonium bromide titan yellow carries out titration colour developing, obtains the mass content of the cetyl trimethyl ammonium bromide remained, then retrodicts and obtain the content of 4-propyl bromide; Measure the massfraction of the waste liquid of different dilution ratio, and carry out contrast correction with the pure 4-propyl bromide volumetric molar concentration curve recorded in advance, thus obtain 4-propyl bromide volumetric molar concentration in waste liquid.
Beneficial effect: compared with prior art, advantage of the present invention is: by setting up the linearity curve A of pure 4-propyl bromide volumetric molar concentration, by adding the 4-propyl bromide of known quantity to waste liquid to be measured, then recurrence correction is carried out to its test result, thus to eliminate in waste liquid impurity to the impact of titration effect, obtain the exact level of 4-propyl bromide in waste liquid, analysis precision can reach more than 95%, and repeatability is high, meet the requirement of 4-propyl bromide content in quantitative determination zeolite synthesis waste liquid, thus waste liquid is reused.
Accompanying drawing explanation
Accompanying drawing is longitudinally to be titrated to the quality of the cetyl trimethyl ammonium bromide solution that terminal consumes, the horizontal coordinate system set up with the volumetric molar concentration of 4-propyl bromide, and draw the linearity curve that obtains of point diagram in a coordinate system, ■ is linearity curve A, and zero is linearity curve (B
1..., B
n), ● be linearity curve C.
Embodiment
Below in conjunction with the drawings and specific embodiments, illustrate the present invention further, these embodiments should be understood only be not used in for illustration of the present invention and limit the scope of the invention, after having read the present invention, the amendment of those skilled in the art to the various equivalent form of value of the present invention has all fallen within the application's claims limited range.
The quantitative determination method of 4-propyl bromide content in zeolite synthesis waste liquid, specifically comprises the following steps:
Step (1) draws the linearity curve A of pure 4-propyl bromide volumetric molar concentration:
A () pipettes the pure 4-propyl bromide solution of 5mL concentration known, be placed in 250mL volumetric flask, with distilled water diluting to scale; Pipette pure 4-propyl bromide solution, the volume V after 5mL dilution
1for 5mL concentration c
1for the tetraphenylboron sodium standard solution of 0.01mol/L, be placed in conical flask, then add 5mL formaldehyde, the NaOH solution of 0.2mL massfraction 20%, the titan yellow indicator solution of 1mL massfraction 0.1%, use concentration c
2for the cetyl trimethyl ammonium bromide solution of 0.01mol/L is titrated to terminal, consume volume V
2;
The calculating formula of 4-propyl bromide massfraction can be obtained thus, i.e. formula 1. w=50 × (c
1v
1-c
2v
2) × M × 100%/W, wherein M is 4-propyl bromide molal weight, W is 4-propyl bromide quality;
Wherein, tetraphenylboron sodium standard solution can also be prepared by the following method, better measures effect to reach: get aluminium choride 1.0g, is dissolved in 25mL water, and constantly stirring and slowly drip sodium hydroxide solution is 8 ~ 9 to pH value, obtains gel aluminum hydroxide; Get tetraphenylboron sodium 3.5g, the 50mL jolting that adds water makes it to dissolve, and adds described gel aluminum hydroxide 12.5mL, jolts 5 minutes, add sodium chloride 8.3g, fully stir evenly, add water 250mL jolting 15 minutes, leaves standstill 10 minutes, filter with double-deck Medium speed filter paper, dripping sodium hydroxide solution to pH value in filtrate is 8 ~ 9, then is diluted with water to 1000mL and shakes up, and to obtain final product.
B () repeats (a), test the pure 4-propyl bromide solution of multiple different concentration known respectively.
C () as shown in drawings, longitudinally to be titrated to the quality of the cetyl trimethyl ammonium bromide solution that terminal consumes, the horizontal coordinate system set up with the volumetric molar concentration of 4-propyl bromide, point diagram is drawn in a coordinate system with the test result of (a) and (b), and through linear regression, obtain the linearity curve A of pure 4-propyl bromide volumetric molar concentration;
The equation of this linearity curve A is y=4.878 × x-0.0000851271, and wherein the y quality that is the cetyl trimethyl ammonium bromide solution that is titrated to terminal and consumes, x are the volumetric molar concentration of pure 4-propyl bromide.
Step (2) draws the linearity curve (B of 4-propyl bromide volumetric molar concentration in waste liquid
1..., B
n):
D () pipettes 5mL waste liquid, with distilled water diluting 50 times; Pipette described waste liquid, the pure 4-propyl bromide solution of known quality and the tetraphenylboron sodium standard solution of 5mL concentration 0.01mol/L after 5mL dilution, be placed in conical flask, add 5mL formaldehyde, the NaOH solution of 0.2mL massfraction 20%, the titan yellow indicator solution of 1mL massfraction 0.1% again, be titrated to terminal with the cetyl trimethyl ammonium bromide solution of concentration 0.01mol/L.
E () repeats (d), by described waste liquid dilution different multiplying, test respectively.
F () as shown in drawings, in the coordinate system, with the test result of (d), (e), namely draw point diagram with the volumetric molar concentration of 4-propyl bromide in the quality being titrated to the cetyl trimethyl ammonium bromide solution that terminal consumes and the waste liquid estimated, obtain the linearity curve (B of the 4-propyl bromide volumetric molar concentration of waste liquid under different dilution ratio
1..., B
n), in the waste liquid estimated, the volumetric molar concentration of 4-propyl bromide refers to the volumetric molar concentration of 4-propyl bromide in the waste liquid recorded by other method, such as ion isolation process, adopt ICS-1000 type ion chromatograph, common cationic exchange chromatography post is selected to be separating column, mobile phase is methyl sulfonic acid, and flow velocity is 1.0mL/min.
Step (3) modified line linearity curve (B
1..., B
n): as shown in drawings, for the waste liquid that dilution ratio is little, its linearity curve slope is large, the waste liquid that dilution ratio is large, and its linearity curve slope is little; According to linearity curve (B
1..., B
n) slope, linear regression is carried out to what differ greatly with linearity curve A slope, the volumetric molar concentration of 4-propyl bromide in the waste liquid estimated is multiplied by correction factor revised, until the slope of revised linearity curve is consistent with A slope, with slope error be no more than ± 0.02% be weigh the consistent standard of slope, the linearity curve C being 4-propyl bromide volumetric molar concentration in quantitative determination waste liquid obtained;
Correction factor refers to linearity curve (B
1..., B
n) ratio of slope of respective slope and linearity curve A.
4-propyl bromide content in step (4) quantitative determination zeolite synthesis waste liquid: for certain waste liquid to be measured, according to linearity curve C, by quality waste liquid being titrated to the cetyl trimethyl ammonium bromide solution that terminal consumes, can obtain the volumetric molar concentration of 4-propyl bromide in waste liquid, more 1. through type can calculate the content of 4-propyl bromide in waste liquid.
The linearity curve C of the present invention by obtaining, can determine 4-propyl bromide content in zeolite synthesis waste liquid fast, quantitatively, accurately.
Owing to usually containing NaOH and a large amount of SiO in zeolite synthesis waste liquid
2the impurity such as solid granule, therefore adopt the mixed solution of silicasol, NaOH and 4-propyl bromide to carry out waste liquid component that is virtually reality like reality, SiO in this mixed solution
2massfraction is 8%, NaOH massfraction is 2%, 4-propyl bromide massfraction is respectively 1%, 2%, 4%, 8%.According to the inventive method and the linearity curve C that obtains, 4 parts of mixed solutions are measured respectively, obtain following result:
As can be seen here, the estimating precision of the inventive method can reach more than 95%, can the content of 4-propyl bromide in Accurate Determining waste liquid.
Claims (3)
1. zeolite synthesizes the quantitative determination method of 4-propyl bromide content in waste liquid, it is characterized in that specifically comprising the following steps:
Step (1) draws the linearity curve A of pure 4-propyl bromide volumetric molar concentration:
A () pipettes the pure 4-propyl bromide solution of 5mL concentration known, with distilled water diluting 50 times; Pipette the tetraphenylboron sodium standard solution of the described pure 4-propyl bromide solution after 5mL dilution, 5mL concentration 0.01mol/L, be placed in conical flask, add 5mL formaldehyde, the NaOH solution of 0.2mL massfraction 20%, the titan yellow indicator solution of 1mL massfraction 0.1% again, be titrated to terminal with the cetyl trimethyl ammonium bromide solution of concentration 0.01mol/L;
B () repeats (a), test the pure 4-propyl bromide solution of multiple different concentration known respectively;
C () is set up coordinate system with the quality of cetyl trimethyl ammonium bromide solution being titrated to terminal and consuming and the volumetric molar concentration of pure 4-propyl bromide solution and is drawn point diagram, obtain linearity curve A and the equation y=4.878 × x-0.0000851271 thereof of pure 4-propyl bromide volumetric molar concentration, wherein the y quality that is the cetyl trimethyl ammonium bromide solution that is titrated to terminal and consumes, x are the volumetric molar concentration of pure 4-propyl bromide;
Step (2) draws the linearity curve (B of 4-propyl bromide volumetric molar concentration in waste liquid
1..., B
n):
D () pipettes 5mL waste liquid, with distilled water diluting 50 times; Pipette described waste liquid, the pure 4-propyl bromide solution of known quality and the tetraphenylboron sodium standard solution of 5mL concentration 0.01mol/L after 5mL dilution, be placed in conical flask, add 5mL formaldehyde, the NaOH solution of 0.2mL massfraction 20%, the titan yellow indicator solution of 1mL massfraction 0.1% again, be titrated to terminal with the cetyl trimethyl ammonium bromide solution of concentration 0.01mol/L;
E () repeats (d), by described waste liquid dilution different multiplying, test respectively;
F () is set up coordinate system with the volumetric molar concentration of 4-propyl bromide in the quality of the cetyl trimethyl ammonium bromide solution being titrated to terminal and consuming and the waste liquid estimated and is drawn point diagram, obtain the linearity curve (B of the 4-propyl bromide volumetric molar concentration of waste liquid under different dilution ratio
1..., B
n);
Step (3) modified line linearity curve (B
1..., B
n): by by (B
1..., B
n) linear regression, obtain being no more than with A slope error ± the linearity curve C of 0.02% is the linearity curve of 4-propyl bromide volumetric molar concentration in quantitative determination waste liquid;
4-propyl bromide content in step (4) quantitative determination zeolite synthesis waste liquid: for certain waste liquid to be measured, according to linearity curve C, by the quality being titrated to the cetyl trimethyl ammonium bromide solution that terminal consumes, 4-propyl bromide content in waste liquid can be obtained.
2. zeolite according to claim 1 synthesizes the quantitative determination method of 4-propyl bromide content in waste liquid, it is characterized in that: contained by described zeolite synthesis waste liquid, component comprises SiO
2solid particle, NaOH, 4 bromide.
3. zeolite according to claim 1 synthesizes the quantitative determination method of 4-propyl bromide content in waste liquid, it is characterized in that: described tetraphenylboron sodium standard solution is prepared by the following method: get aluminium choride 1.0g, be dissolved in 25mL water, it is 8 ~ 9 to pH value that continuous stirring also slowly drips sodium hydroxide solution, obtains gel aluminum hydroxide; Get tetraphenylboron sodium 3.5g, the 50mL jolting that adds water makes it to dissolve, and adds described gel aluminum hydroxide 12.5mL, jolts 5 minutes, add sodium chloride 8.3g, fully stir evenly, add water 250mL jolting 15 minutes, leaves standstill 10 minutes, filter with double-deck Medium speed filter paper, dripping sodium hydroxide solution to pH value in filtrate is 8 ~ 9, then is diluted with water to 1000mL and shakes up, and to obtain final product.
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| CN104237219B (en) * | 2014-08-20 | 2016-08-24 | 浙江大学 | A kind of water quality quaternary ammonium salt semi-quantitative detection method |
| CN109160881B (en) * | 2018-10-31 | 2021-01-08 | 江西肯特化学有限公司 | Method for extracting tetrapropylammonium bromide from zeolite synthesis waste liquid |
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Address after: 212000 No. 90 Chenglu Road, new town, Zhenjiang, Jiangsu Patentee after: Jiangsu guoci New Material Technology Co., Ltd Address before: 212000, 90, Cheng Cheng Road, Zhenjiang New District, Jiangsu, Zhenjiang Patentee before: JIANGSU GUOCI TIANNUO NEW MATERIAL TECHNOLOGY Co.,Ltd. |
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