CN101358928B - Method for measuring solid amines catalyst for roof liner of automobile - Google Patents

Abstract

The present invention relates to a determination method of solid amine catalyst which is used in the top linear of a vehicle, belonging to the technical field of quantitative analysis. The method adopts principles of the color changing of acidic indicators and the acid-alkali neutralization, so as to accurately determine the concentration of the solid amine catalyst in the solution, and comprisesthe following steps: firstly, hydrochloric acid solution and bromocresol green-methyl red are prepared, and the hydrochloric acid solution is calibrated; secondly, the hydrochloric acid solution is used for calibrating the concentration of the catalyst used on the site, and the color changing of the selected phenolphthalein indicator and the used amount of the standard hydrochloric acid solutionare applied to calculate the actual concentration of the catalyst used on the site; thirdly, the actual determination results are applied to judge whether the solid amine catalyst satisfies the production requirements; if the solid amine catalyst does not satisfy the production requirements, the concentration of the catalyst is readjusted so that the solid amine catalyst satisfies the production requirements. The method has the advantages of simple operation, stable testing results and short testing time. Simultaneously, the testing equipment is simple and easy to purchase. And the method is suitable for wide application in the internal decorating industry of vehicles.

Description

The assay method of solid amines catalyst for roof liner of automobile

Technical field

The present invention relates to the assay method of solid amines catalyst for roof liner of automobile, specifically utilize the stability of spraying catalyzer in the glue link in the chemical analysis gimmick testing automobile interior trim process industry, belong to the quantitative analysis tech field.

Background technology

Auto manufacturing is rapid in Development in China, and the development of thing followed parts also adds on a large scale.The production technology that present domestic most of automobile roof liner manufacturing enterprise adopts is a dry process, be exactly to utilize compound substance and lining to carry out compound suppressing to produce roof liner in simple terms, this worker's method exists: the raw materials cost height, many defectives such as component end item acoustical behavior difference, under the more and more fierce situation of car industry competition at present, adopt a kind of raw material low cost, the production technology that end properties is high will certainly become development trend.Worker's method is in the field of business is referred to as for this: wet processing, its fundamental point is to adopt primary material to carry out compound and processing, may satisfy the requirement of different performance roof liner by the combination that changes material, in this technology, the binder that uses is particularly important, binder has not only played the adhesive effect between material and the material, simultaneously, can produce very big influence for the rigidity and the acoustics of product.

Because the requirement of environment-protecting industrial at present, the glue that adopts must be asepsis environment-protecting glue, therefore, it is optimum and appropriate using the glue of PU class, simultaneously, PU class glue in use, need to use the catalyzer of stabilized formulations to trigger its reaction moulding, the catalyst concentration instability can cause the speed in the reaction time of glue, can influence the whole production link, therefore, the steady concentration of assurance catalyzer is even more important.

Traditional solution concentration assay method is to add thermal crystalline, uses balance to weigh after the quality of solution and crystal, draws the concentration of solution according to solution quality on the solute mass ratio.This method is simple, but method itself is subjected to the restriction of solute physical characteristics.For volatile, fusing point is low, low-boiling material, heating-up temperature is too high, causes solute volatilization or chemical change takes place, and measurement can't be carried out.

This method directly adopts the solution of actual catalyst to carry out on-site measurement, need not catalyzer is carried out any pre-service and processing, directly experimentize, method is easy, process is simple and practical, and result of calculation is accurate, and than adopting high most advanced and sophisticated experimental facilities analysis, with low cost, have extensive operability and practicality that factory uses.

Commercial production needs the scene that catalyzer is carried out management and control, the content of guaranteeing catalyzer is in stable scope, could guarantee the production that product is stable, if adopting high-end liquid chromatography device to detect tests at the scene, maintenance and use for liquid chromatography device lack management and control, simultaneously, and liquid chromatography device detecting operation complexity, the time that needs is longer, can not obtain a result fast.

Summary of the invention

The objective of the invention is to overcome above-mentioned weak point, thereby provide a kind of easy and simple to handle, detect with low cost, the testing result good stability, be suitable for the on-the-spot method that detects of using of factory, this method adopts the principle of acid indicator variable color and acid-base neutralization, accurately the concentration of the solid amine of test solution neutral and alkali material.

Main solution of the present invention is achieved in that

Method of testing step of the present invention is as follows:

A, according to operating position, prepare corresponding HCl volumetric solution, volumetric solution is used in to be measured catalyzer, the mensuration of catalyst concn characterizes out by volumetric solution.

B, accurately prepare corresponding indicator solution, select suitable indicator, use interval and scope to guarantee variable color.

C, according to the HCl solution of step a, select the corresponding standard alkaline solution that the HCl solution that step a is produced is demarcated.

D, carry out data processing, obtain the concrete concentration C of the HCl solution of corresponding step a according to the resulting result of step c _All, at this moment, the concentration of HCl solution is determined, keeps the HCl solution of corresponding step a, as the known calibration solution use of catalyzer.

E, accurately prepare in the solution to be measured known to the different aqueous solution of concentration more than 3 parts or 3 parts of solute.

F, accurate every kind of variable concentrations of weighing sample solution M to be tested _{To be measured}, use indicator to splashing into 3～4 in its solution, the sample that draws produces variable color, the HCl solution that use a step to be prepared this moment carries out titration to sample, when titration till the native color, the HCl solution amount V that a step that record is consumed is prepared.

G, according to equimolar principle, experimental formula V _HCl=(C _All* V)/0.1157 draw corresponding V _HCl

H, the corresponding M that obtains more than the basis _{To be measured}, V _HClWith the concentration for preparing solution, use the origin software of U.S. OriginLab company (its predecessor is Microcal company) exploitation to set up typical curve and simulate computing formula;

I, the sample of concentration to be tested is carried out weighing draw M _{To be measured}

J, the HCl volumetric solution amount that the titration process of unknown sample consumes, the substitution experimental formula obtains V _HCl

K, M _{To be measured}, V _HClGo in the formula that substitution step h is produced, obtain the concentration of corresponding unknown solution.

Wherein, step e accurately in the preparation solution to be measured known to the aqueous solution of solute be 3～7 parts.

Step a-d is the calibration process of HCl volumetric solution, if use this volumetric solution, need carry out calibration experiment once more and redefine C _All

Technical scheme of the present invention: a kind of assay method of solid amines catalyst for roof liner of automobile, the principle of employing acid indicator variable color and acid-base neutralization, the accurately concentration of solid amines catalyst in the test solution;

(1) preparation hydrochloric acid standard solution and bromcresol green-methyl red indicator carry out the demarcation of hydrochloric acid standard solution;

(2) use hydrochloric acid standard solution to demarcate the on-the-spot catalyst concentration of using, the variable color by adopting selected phenolphthalein indicator and the use amount of hydrochloric acid standard solution are by calculating the actual concentrations of confirming the on-the-spot catalyzer that uses; Method is:

1. the concentration of amine is the concentration determination of the solid amine of low concentration of 4%-10% admittedly:

Accurate weighing M _{To be measured}Catalyst sample is accurate to 0.001g, the M that takes by weighing _{To be measured}Be controlled at 5g, place Erlenmeyer flask; The catalyst sample that takes by weighing is diluted to the solution of 70mL with deionized water; Splash into 3～4 0.1% phenolphthalein indicators, solution colour becomes aubergine by water white transparency; Adopt calibrated hydrochloric acid standard solution that sample is carried out titration, titration to solution colourless till, and write down the volume V of used hydrochloric acid standard solution;

Formula: V rule of thumb _HCl=(C _All* V)/0.1157, obtain corresponding V _HCl, C in the formula _AllConcentration for hydrochloric acid standard solution;

Data processing: handle above operation by application software origin and draw data, draw corresponding curve map and fitting formula automatically, and formula is simplified, thereby draw:

The relative concentration of solid amine in the solution:

C _Sample%=0.30743+1.34869 (V _HCl/ M _{To be measured}) 1.;

2. the concentration of amine is the concentration determination of the solid amine of middle concentration of 10%-20% admittedly:

Accurate weighing M _{To be measured}Catalyst sample is accurate to 0.001g, the M that takes by weighing _{To be measured}Be controlled at 2g, place Erlenmeyer flask; The catalyst sample that takes by weighing is diluted to the solution of 70mL with deionized water; Splash into 3～4 0.1% phenolphthalein indicators, solution colour becomes aubergine by water white transparency; Adopt calibrated hydrochloric acid standard solution that sample is carried out titration, titration to solution colourless till, and write down the volume V of used hydrochloric acid standard solution;

Formula: V rule of thumb _HCl=(C _All* V)/0.1157, obtain corresponding V _HCl, C in the formula _AllConcentration for hydrochloric acid standard solution;

Data processing: handle above operation by application software origin and draw data, draw corresponding curve map and fitting formula automatically, and formula is simplified, thereby draw:

The relative concentration of solid amine in the solution:

C _Sample%=0.29326+1.33520 (V _HCl/ M _{To be measured}) 2.;

3. the concentration of amine is the concentration determination of the solid amine of high concentration of 20%-35% admittedly:

Accurate weighing M _{To be measured}Catalyst sample is accurate to 0.001g, the M that takes by weighing _{To be measured}Be controlled at 2g, place Erlenmeyer flask; The catalyst sample that takes by weighing is diluted to the solution of 70mL with deionized water; Splash into 3～4 0.1% phenolphthalein indicators, solution colour becomes aubergine by water white transparency; Adopt calibrated hydrochloric acid standard solution that sample is carried out titration, titration to solution colourless till, and write down the volume V of used hydrochloric acid standard solution;

Formula: V rule of thumb _HCl=(C _All* V)/0.1157, obtain corresponding V _HCl, C in the formula _AllConcentration for hydrochloric acid standard solution;

Data processing: handle above operation by application software origin and draw data, draw corresponding curve map and fitting formula automatically, and formula is simplified, thereby draw:

The relative concentration of solid amine in the solution:

C _Sample%=0.31275+1.34319 (V _HCl/ M _{To be measured}) 3.;

(3) measurement result according to reality judges whether to meet production requirement, if do not meet, will readjust the requirement that catalyst concentration reaches production.

Beneficial effect of the present invention: this method has characteristics such as easy and simple to handle, quick, favorable reproducibility, analysis time be short, and this method not only applicable to volatile, fusing point is low, the solution concentration of low-boiling material is measured but also applicable to the solution concentration mensuration of difficulty volatilization, fusing point height, material that boiling point is high.

Embodiment

Common segment

1, the HCl of the preparation of hydrochloric acid volumetric solution: 9mL (dense) is dissolved in the 1000mL water, uses volumetric flask fixed molten.Glasswares such as volumetric flask, beaker, glass bar need use deionized water to clean wall of cup, put into baking oven and dry 1h.

2, the preparation of bromcresol green-methyl red indicator: be about 0.1g bromcresol green+0.02g methyl red, be dissolved in the ethanol of 100mL95%, because indicator is the effect of playing discoloration indication,, therefore adopts valuation to add and get final product for the obvious requirement of how much not having of addition.

3, hydrochloric acid solution is demarcated: use oven for drying sodium carbonate solid, need oven dry 2h, with the dry no moisture of the material that guarantees to adopt, the result is not exerted an influence; Use a certain amount of sodium carbonate of Erlenmeyer flask weighing (M), use deionized water that it is dissolved, after solid matter dissolves fully, stop to add deionized water; Add 2-3 and drip bromcresol green-methyl red indicator in this Erlenmeyer flask, sodium carbonate liquor becomes green; Use that hydrochloric acid solution to be calibrated carries out titration experiments to sodium carbonate liquor in the volumetric flask, titration to sodium carbonate liquor moment becomes till the kermesinus, and the consumption of record hydrochloric acid is V _HClRepeat to test 3 times, obtain 4 groups of V _HCl

4, concentration of hydrochloric acid calculates: the formula that the principle by equimolar amounts draws:

C _HCl＝(M×2×1000)/106×V _HCl

Draw corresponding C _HCIProcessing draws mean value C _AllAt the enterprising line identifier of volumetric flask.

The concentration determination of embodiment 1, the solid amine of low concentration

1, use the solid amine of the accurate weighing of electronic balance, the configuration quality percent concentration is respectively 5 kinds of solution of 4.25%, 5.25%, 6.25%, 7.25%, 8.25%.

2, the mensuration of solid amines catalyst concentration: accurate weighing M _{To be measured}Catalyst sample (is accurate to 0.001g, the M that takes by weighing _{To be measured}Be controlled at about 5g) to Erlenmeyer flask; Use deionized water that it is diluted to about 70mL; Splash into 3-4 0.1% phenolphthalein indicators, color sample becomes aubergine by water white transparency; Adopt calibrated hydrochloric acid solution that sample is carried out titration, titration and is write down the volume V of used hydrochloric acid standard solution till colourless;

Formula: V rule of thumb _HCl=(C _All* V)/0.1157, obtain corresponding V _HCl

3, data processing: handle above operation by application software origin and draw data, automatically draw corresponding curve map and fitting formula, and to formula as suitable simplification, thereby draw: the relative concentration of solution: C% (sample)=0.30743+1.34869 (V _HCl/ M _{To be measured}) 1.

4, according to the empirical value substitution expression formula in the table 1 1. in, obtain corresponding calculating solubility, calculating concentration and the actual concentrations that obtains contrasted to verify the rationality of this expression formula, comparing result sees Table 2.

Table 1

Gu the concentration of amine aqueous solution	4.25	5.25	6.25	7.25	8.25
						V HCL/M To be measured	2.98	3.71	4.41	5.17	5.89
The acid titrimetry records V HCL	14.95	18.58	22.1	25.9	29.5
						Grammes per square metre (M To be measured)	5.0253	5.0147	5.0093	5.009	5.0064

Table 2

Actual concentrations	Calculating concentration	Error
			4.25％	4.32％	0.07％
5.25％	5.31％	0.06％
			6.25％	6.26％	0.01％
7.25％	7.28％	0.03％
			8.25％	8.25％	0.00％

Correlation data finds that test and the resulting formula of software match are adapted at the test use of the solid amine of low concentration by experiment.

The concentration determination of embodiment 2, the solid amine of middle concentration

1, use the solid amine of the accurate weighing of electronic balance, the configuration quality percent concentration is respectively 5 kinds of solution of 12%, 13%, 14%, 15%, 16%.

2, the mensuration of solid amines catalyst concentration: accurate weighing M _{To be measured}Catalyst sample (is accurate to 0.001g, the M that takes by weighing _{To be measured}Be controlled at about 2g) to Erlenmeyer flask; Use deionized water that it is diluted to about 70mL; Splash into 3～4 0.1% phenolphthalein indicators, color sample becomes aubergine by water white transparency; Adopt calibrated hydrochloric acid solution that sample is carried out titration, titration and is write down the volume V of used hydrochloric acid standard solution till colourless;

Formula: V rule of thumb _HCl=(C _All* V)/0.1157, obtain corresponding V _HCl

3, data processing: handle above operation by application software origin and draw data, draw corresponding curve map and fitting formula automatically, and to formula as suitable simplification, thereby draw:

The relative concentration of solution: C% (sample)=0.29326+1.33520 (V _HCl/ M _{To be measured}) 2.

4, according to the empirical value substitution expression formula in the table 3 2. in, obtain corresponding calculating solubility, calculating concentration and the actual concentrations that obtains contrasted to verify the rationality of this expression formula, comparing result sees Table 4.

Table 3

The concentration of softening water	12	13	14	15	16
						V HCL/M To be measured	8.78	9.52	10.25	10.91	11.69
The acid titrimetry records V HCL	17.85	19.1	20.51	21.97	23.63
						Grammes per square metre (M To be measured)	2.0327	2.0056	2.0017	2.0145	2.0212

Table 4

Actual concentrations	Calculating concentration	Error
			12％	12.02％	0.02％
13％	13.01％	0.01％
			14％	13.97％	-0.03％
15％	14.86％	-0.14％
			16％	15.90％	-0.10％

Correlation data finds that test and the resulting formula of software match are adapted at the test use of the solid amine of middle concentration by experiment.

The concentration determination of embodiment 3, the solid amine of high concentration

1, use the solid amine of the accurate weighing of electronic balance, the configuration quality percent concentration is respectively 5 kinds of solution of 25%, 27%, 29%, 31%, 33%.

2, the mensuration of solid amines catalyst concentration: accurate weighing M _{To be measured}Catalyst sample (is accurate to 0.001g, the M that takes by weighing _{To be measured}Be controlled at about 2g) to Erlenmeyer flask; Use deionized water that it is diluted to about 70ml; Splash into 3～4 0.1% phenolphthalein indicators, color sample becomes aubergine by water white transparency; Adopt calibrated hydrochloric acid solution that sample is carried out titration, titration and is write down the volume V of used hydrochloric acid standard solution till colourless;

Formula: V rule of thumb _HCl=(C _All* V)/0.1157, obtain corresponding V _HCl

3, data processing: handle above operation by application software origin and draw data, automatically draw corresponding curve map and fitting formula, and to formula as suitable simplification, thereby draw: the relative concentration of solution: C% (sample)=0.31275+1.34319 (V _HCl/ M _{To be measured}) 3.

4, according to the empirical value substitution expression formula in the table 5 3. in, obtain corresponding calculating solubility, calculating concentration and the actual concentrations that obtains contrasted to verify the rationality of this expression formula, comparing result sees Table 6.

Table 5

The concentration of softening water	25	27	29	31	33
						V HCL/M To be measured	18.42	19.8	21.25	22.92	24.34
The acid titrimetry records V HCL	37.53	40.05	43.73	46.21	48.97
						Grammes per square metre (M To be measured)	2.038	2.0224	2.0577	2.0164	2.0125

Table 6

Actual concentrations	Calculating concentration	Error
			25％	25.05％	0.05％

Actual concentrations	Calculating concentration	Error
			27％	26.91％	-0.09％
29％	28.85％	-0.15％
			31％	31.10％	0.10％
33％	33.01％	0.01％

Correlation data finds that test and the resulting formula of software match are adapted at the test use of the solid amine of high concentration by experiment.

Claims (1)

1. an automobile roof liner is characterized in that adopting the principle of acid indicator variable color and acid-base neutralization, accurately the concentration of solid amine catalyst in the test solution with the assay method of solid amine catalyst;

(1) preparation hydrochloric acid standard solution and bromcresol green-methyl red indicator carry out the demarcation of hydrochloric acid standard solution;

(2) use hydrochloric acid standard solution to demarcate the on-the-spot catalyst concentration of using, the variable color by adopting selected phenolphthalein indicator and the use amount of hydrochloric acid standard solution are by calculating the actual concentrations of confirming the on-the-spot catalyzer that uses; Method is:

1. the concentration of amine is the concentration determination of the solid amine of low concentration of 4%-10% admittedly:

Accurate weighing M _{To be measured}Catalyst sample is accurate to 0.001g, the M that takes by weighing _{To be measured}Be controlled at 5g, place Erlenmeyer flask; The catalyst sample that takes by weighing is diluted to the solution of 70mL with deionized water; Splash into 3～4 0.1% phenolphthalein indicators, solution colour becomes aubergine by water white transparency; Adopt calibrated hydrochloric acid standard solution that sample is carried out titration, titration to solution colourless till, and write down the volume V of used hydrochloric acid standard solution;

Formula: V rule of thumb _HCl=(C _All* V)/0.1157, obtain corresponding V _HCl, C in the formula _AllConcentration for hydrochloric acid standard solution;

Data processing: handle above operation by application software origin and draw data, draw corresponding curve map and fitting formula automatically, and formula is simplified, thereby draw:

The relative concentration of solid amine in the solution:

C _Sample%=0.30743+1.34869 (V _HCl/ M _{To be measured}) 1.;

2. the concentration of amine is the concentration determination of the solid amine of middle concentration of 10%-20% admittedly:

Accurate weighing M _{To be measured}Catalyst sample is accurate to 0.001g, the M that takes by weighing _{To be measured}Be controlled at 2g, place Erlenmeyer flask; The catalyst sample that takes by weighing is diluted to the solution of 70mL with deionized water; Splash into 3～4 0.1% phenolphthalein indicators, solution colour becomes aubergine by water white transparency; Adopt calibrated hydrochloric acid standard solution that sample is carried out titration, titration to solution colourless till, and write down the volume V of used hydrochloric acid standard solution;

Formula: V rule of thumb _HCl=(C _All* V)/0.1157, obtain corresponding V _HCl, C in the formula _AllConcentration for hydrochloric acid standard solution;

Data processing: handle above operation by application software origin and draw data, draw corresponding curve map and fitting formula automatically, and formula is simplified, thereby draw:

The relative concentration of solid amine in the solution:

C _Sample%=0.29326+1.33520 (V _HCl/ M _{To be measured}) 2.;

3. the concentration of amine is the concentration determination of the solid amine of high concentration of 20%-35% admittedly:

Accurate weighing M _{To be measured}Catalyst sample is accurate to 0.001g, the M that takes by weighing _{To be measured}Be controlled at 2g, place Erlenmeyer flask; The catalyst sample that takes by weighing is diluted to the solution of 70mL with deionized water; Splash into 3～4 0.1% phenolphthalein indicators, solution colour becomes aubergine by water white transparency; Adopt calibrated hydrochloric acid standard solution that sample is carried out titration, titration to solution colourless till, and write down the volume V of used hydrochloric acid standard solution;

Formula: V rule of thumb _HCl=(C _All* V)/0.1157, obtain corresponding V _HCl, C in the formula _AllConcentration for hydrochloric acid standard solution;

Data processing: handle above operation by application software origin and draw data, draw corresponding curve map and fitting formula automatically, and formula is simplified, thereby draw:

The relative concentration of solid amine in the solution:

C _Sample%=0.29326+1.33520 (V _HCl/ M _{To be measured}) 2.;

3. the concentration of amine is the concentration determination of the solid amine of high concentration of 20%-35% admittedly:

Accurate weighing M _{To be measured}Catalyst sample is accurate to 0.001g, the M that takes by weighing _{To be measured}Be controlled at 2g, place Erlenmeyer flask; The catalyst sample that takes by weighing is diluted to the solution of 70mL with deionized water; Splash into 3～4 0.1% phenolphthalein indicators, solution colour becomes aubergine by water white transparency; Adopt calibrated hydrochloric acid standard solution that sample is carried out titration, titration to solution colourless till, and write down the volume V of used hydrochloric acid standard solution;

Formula: V rule of thumb _HCl=(C _All* V)/0.1157, obtain corresponding V _HCl, C in the formula _AllConcentration for hydrochloric acid standard solution;

Data processing: handle above operation by application software origin and draw data, draw corresponding curve map and fitting formula automatically, and formula is simplified, thereby draw:

The relative concentration of solid amine in the solution:

C _Sample%=0.31275+1.34319 (V _HCl/ M _{To be measured}) 3.;

(3) measurement result according to reality judges whether to meet production requirement, if do not meet, will readjust the requirement that catalyst concentration reaches production.