Pre-reaction liquid for chlorinated rubber adhesive and preparation method of pre-reaction liquid

A technology of chlorinated rubber and adhesives, which is applied in the direction of halogen rubber derivative adhesives, adhesives, adhesive types, etc., and can solve problems such as solid-liquid delamination that is not easy to occur

Active Publication Date: 2021-12-14

NANJING FORESTRY UNIV

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AI-Extracted Technical Summary

Problems solved by technology

[0003] In order to solve the problems existing in the prior art, the present invention provides a pre-reaction...

Abstract

The invention provides a pre-reaction liquid for a chlorinated rubber adhesive and a preparation method thereof.The pre-reaction liquid is prepared through the following steps: magnesium nitrate and aluminum nitrate are used for preparing magnesium-aluminum hydrotalcite, then a layered-embedded hydrotalcite-sodium phenolate compound is prepared, the hydrotalcite-sodium phenolate compound firstly coats the surfaces of magnesium oxide particles, then, high-molecular-weight p-tert-butylphenol formaldehyde resin can be adsorbed on the surfaces of the magnesium oxide particles, so that the magnesium oxide particles in the pre-reaction liquid suspend in the solution and are not easy to agglomerate to form precipitates, and the solid-liquid layering phenomenon of the pre-reaction liquid is prevented. The prepared pre-reaction liquid can be applied to preparation of an adhesive for chlorinated rubber, the adhesive force, heat resistance and storage stability of the adhesive are improved, and the pre-reaction liquid is easy to prepare and suitable for popularization and application.

Application Domain

Non-macromolecular adhesive additivesAldehyde/ketone condensation polymer adhesives +2

Technology Topic

Magnesium nitrateAdhesive cement +6

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Examples

Experimental program(5)
Comparison scheme(4)
Effect test(2)

Example Embodiment

[0029] Example 1

[0030] A chlorinated rubber adhesive with a pre-reaction solution, which was prepared following steps:

[0031] (1) Distilled water at room temperature of aluminum nitrate nonahydrate, magnesium nitrate hexahydrate and removing carbon dioxide mixing, the resulting mixture at a speed of 100r / min of stirring the pH was adjusted to 7.0 with lye, and then under nitrogen the reaction 0.5h stirring speed of 500r / min, the resulting reaction mixture was placed in a sealed reaction vessel gum at 70 ℃ 2h, the resulting mixture was filtered, and washed with distilled water until the filtrate was neutral to remove carbon dioxide, filtered out alternate thereof; step (1) in the lye employed 5wt% NaOH solution, magnesium hexahydrate step (1) nitrate, aluminum nitrate nonahydrate and removing carbon dioxide and water of the weight ratio of 1: 0.32: 15;

[0032] (2) A solution obtained in step a gum, sodium phenoxide, removing mixing carbon dioxide with distilled water, then filtered in a nitrogen atmosphere and reacting the product 10h at a speed of 200r / min stirring conditions, obtained, and for the removal of carbon dioxide in distilled water the filtrate was washed until neutral, the precipitate was filtered off and dried at 80 deg.] C 10H, drying the resulting white solid was ground to 300-mesh hydrotalcite - sodium phenoxide standby composite powder; said step (2) obtained in step 1 gum thereof, sodium phenol, carbon dioxide removal distilled three weight ratio of 1: 0.22: 5;

[0033] (3) Step (2) Preparation of hydrotalcite obtained - sodium phenoxide, and magnesium oxide composite powder was added to a mixed solvent of ethyl acetate and cyclohexane, and the resulting mixture was refluxed at 45 ℃ speed of 200r / min with stirring the reaction 3h, then allowed to stand after 12h, to obtain magnesium oxide-containing - hydrotalcite - a solution of sodium phenolate complex; the procedure described in step (2) (3) preparation of hydrotalcite obtained - sodium phenoxide composite powder, oxide magnesium, four of ethyl acetate and cyclohexane by weight ratio of 0.5: 2: 1.2: 20;

[0034] (4) of step (3) is prepared containing magnesia - Hydrotalcite - sodium phenolate complex solution was added tert-butylphenol formaldehyde resin, and the resulting mixture was refluxed at 25 deg.] C at a speed of 200r / min with stirring the reaction 6h, to obtain a chlorinated rubber adhesive with a pre-reaction solution; the procedure described in step (4) (3) preparation the obtained magnesium oxide-containing - hydrotalcite - a solution of sodium phenolate complex and p-tert-butylphenol formaldehyde both resin weight ratio 24:22.

Example Embodiment

[0035] Example 2

[0036] A chlorinated rubber adhesive with a pre-reaction solution, which was prepared following steps:

[0037] (1) Distilled water at room temperature of aluminum nitrate nonahydrate, magnesium nitrate hexahydrate and removing carbon dioxide mixing, the resulting mixture at a speed of 300r / min of stirring the pH was adjusted to 8.0 with lye, and then under nitrogen the reaction 1h stirring speed of 700r / min, the resulting mixture was placed in a reaction 7h at 80 deg.] C in a sealed autoclave, the resultant mixture was filtered, and washed with distilled water until the filtrate became neutral removing carbon dioxide, filtered gum alternate; step (1) in the lye solution using 10wt% NaOH, magnesium hexahydrate step (1) nitrate, aluminum nitrate nonahydrate and removing carbon dioxide and water of the weight ratio of 1.02: 0.34: 18;

[0038] (2) A solution obtained in step a gum, sodium phenoxide, removing mixing carbon dioxide with distilled water, then filtered in a nitrogen atmosphere and reacting the product 20h at a speed of 500r / min stirring conditions, obtained, and for the removal of carbon dioxide in distilled water the filtrate was washed until neutral, the precipitate was filtered off and dried 20h at 90 ℃, dried resulting white solid was ground to 300-mesh hydrotalcite - sodium phenoxide standby composite powder; the (2) obtained in step 1 gum thereof, sodium phenol, carbon dioxide removal distilled three weight ratio of 1: 0.28: 7;

[0039] (3) Step (2) Preparation of hydrotalcite obtained - sodium phenoxide, and magnesium oxide composite powder was added to a mixed solvent of ethyl acetate and cyclohexane, and the resultant mixture at 50 deg.] C at a speed of 1000r / min was stirred at reflux conditions the reaction 3h, then allowed to rest for 18 h, to obtain magnesium oxide-containing - hydrotalcite - a solution of sodium phenolate complex; the procedure described in step (2) (3) preparation of hydrotalcite obtained - sodium phenoxide composite powder, oxide magnesium, four of ethyl acetate and cyclohexane by weight ratio of 0.75: 2.4: 1.4: 25;

[0040] (4) of step (3) is prepared containing magnesia - Hydrotalcite - sodium phenolate complex solution was added tert-butylphenol formaldehyde resin, and the resulting mixture was refluxed at 35 ℃ speed at 500r / min with stirring reaction 7h, to obtain a chlorinated rubber adhesive with a pre-reaction solution; the procedure described in step (4) (3) preparation the obtained magnesium oxide-containing - hydrotalcite - a solution of sodium phenolate complex and p-tert-butylphenol formaldehyde 29:27 weight ratio of the two resins.

Example Embodiment

[0041] Example 3

[0042] A chlorinated rubber adhesive with a pre-reaction solution, which was prepared following steps:

[0043] (1) Distilled water at room temperature of aluminum nitrate nonahydrate, magnesium nitrate hexahydrate and removing carbon dioxide mixing, the resulting mixture at a speed of 550r / min under stirring conditions by alkaline pH was adjusted to 9.5, and then under nitrogen for 2h stirring speed of 1000r / min, and the resulting reaction mixture was placed in a sealed reaction vessel at 100 ℃ 24h, the resulting mixture was filtered, and washed with distilled water until the filtrate became neutral removing carbon dioxide, filtered gum alternate; step (1) in the lye solution using 15wt% NaOH, magnesium hexahydrate step (1) nitrate, aluminum nitrate nonahydrate and removing carbon dioxide and water of the weight ratio of 1.04: 0.37: 22;

[0044] (2) A solution obtained in step a gum, sodium phenoxide, removing mixing carbon dioxide with distilled water, then filtered in a nitrogen atmosphere and reacting the product 30h at a speed of 800r / min stirring conditions, obtained, and for the removal of carbon dioxide in distilled water the filtrate was washed until neutral, the precipitate was filtered off and dried at 100 deg.] C 30h, the solid was dried to give a white ground to 500 mesh hydrotalcite - sodium phenoxide standby composite powder; said step (2) obtained in step 1 gum thereof, sodium phenol, carbon dioxide removal distilled three weight ratio of 1: 0.34: 10;

[0045] (3) Step (2) Preparation of hydrotalcite obtained - sodium phenoxide, and magnesium oxide composite powder was added to a mixed solvent of ethyl acetate and cyclohexane, and the resulting mixture was refluxed at 56 ℃ speed of 1700r / min with stirring the reaction 5h, then allowed to stand after 24h, to obtain magnesium oxide-containing - hydrotalcite - a solution of sodium phenolate complex; the procedure described in step (2) (3) preparation of hydrotalcite obtained - sodium phenoxide composite powder, oxide magnesium, four of ethyl acetate and cyclohexane by weight ratio of 1: 2.9: 1.6: 29;

[0046] (4) of step (3) is prepared containing magnesia - Hydrotalcite - sodium phenolate complex solution was added tert-butylphenol formaldehyde resin, and the resulting mixture was refluxed at 50 deg.] C at a speed of 700r / min with stirring the reaction 8h, to obtain a chlorinated rubber adhesive with a pre-reaction solution; the procedure described in step (4) (3) preparation the obtained magnesium oxide-containing - hydrotalcite - a solution of sodium phenolate complex and p-tert-butylphenol formaldehyde both resin weight ratio 35:31.

[0047] Example of the present embodiment in step (1) X-ray powder diffraction analysis and the sample (2) prepared, in an X-ray powder diffraction is performed on pharmacologically Rigaku D / MAX X-ray diffraction instrument uses Tube voltage 40.0kV, pipe flow 30.0mA), attached test results figure 2 Indicated.

[0048] Attach figure 2 In a step of Example 3 (1) Preparation of gum in powder after drying 48h 100 deg.] C, b is an Example 3 Step (2) Preparation of hydrotalcite - sodium phenolate composite powder. Example 3 Step (1) preparation of the sample after dried gum is characterized Hydrotalcite X-ray diffraction spectrum, X-ray powder diffraction pattern of a diffraction peak representing the hydrotalcite between adjacent plies Layer spacing. Compared with Example 3 Step (1) preparation of a powder sample after drying gum embodiment, the hydrotalcite prepared in Example 3 - the first X-ray powder diffraction peak of sodium phenolate complex moves to the small diffraction angle diffraction direction, DESCRIPTION hydrotalcite - sodium phenolate in phenol complex ions are embedded into the laminate hydrotalcite.

PUM

Property	Measurement	Unit
Thickness	0.2	mm

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