Summary of the invention
Technical problem to be solved by this invention is: reduce the blistered incidence of sponge in the rubber overshoes production process, a kind of sponge bonding and preparation method thereof is provided, this sponge bonding has independently speed on curability, can effectively stop at the bottom of the formation of sponge bubble and the gelatin sponge and the rubber overshoes outer bottom produces layering.The present invention also provides a kind of method that sponge bonding solves sponge bubble at the bottom of the glue of using, this method through rubber technology at one deck sponge bonding of fitting securely at the bottom of the gelatin sponge and between the rubber overshoes outer bottom to prevent its layering.The present invention can make the sponge bubble production rate of rubber overshoes product be in below 0.03%.
The present invention solves rubber overshoes sponge alveolar substance amount problem from the following aspects:
(1) cuts off bonding coat at applying one deck at the bottom of the gelatin sponge and between the rubber overshoes outer bottom, make at the bottom of the gelatin sponge and the rubber overshoes outer bottom sticks together securely, solve at the bottom of the gelatin sponge and the bonding lamination problem of rubber overshoes outer bottom.
(2) at the bottom of making partition bonding coat and gelatin sponge, applying rubber technology sticks together securely.
(3) improve the prescription of sponge bonding, stop the formation of sponge bubble.
The following technical scheme of the concrete employing of the present invention:
According to listed as parts by weight, sponge bonding is to be prepared from for 40~50 parts by 50~150 parts of rubber, 2~3 parts in sulphur, 4~6 parts of vulcanization accelerators, 7~9 parts of vulcanization levellers, 160~210 parts of weighting agents and tackifying resin.
Preferably, sponge bonding is to be prepared from for 45 parts by 100 parts of rubber, 2.5 parts in sulphur, 5 parts of vulcanization accelerators, 8 parts of vulcanization levellers, 185 parts of weighting agents and tackifying resin.
The preparation method of aforementioned sponge bonding: get rubber plasticate make its Wei Shi plasticity number reach 0.40~0.45 broken-(down)rubber, then broken-(down)rubber and sulphur, vulcanization accelerator, vulcanization leveller, weighting agent, tackifying resin are carried out the mixing sponge bonding that promptly gets according to common process.When plasticity number less than 0.4 the time, the rubber unvulcanizate of being refined is rough, sizing material is harder, be easy to generation adhesive glue roll banding phenomenon in the rubber technological process because roller temperature raises, the easy scorching incipient scorch of while adhesive glue, plasticity number was greater than 0.45 o'clock, can produce the sponge bubble, also can paste rubber mixing machine because adhesive glue crosses soft, can not rolling out film.
The present invention also provides two kinds of preferably methods of rubber plastic steelmaking:
Method one: rubber was being descended roll spacing 3~4 times in 40~50 ℃ of machine roller temperatures, condition below the roll spacing 1mm on the opening rubber mixing machine, in the mill of roll spacing 9~10mm, rubber bag roll row is being removed bubble then.
Method two: get the rubber 5~5.5min that plasticates on Banbury mixer, the Banbury mixer condition is: 90~120 ℃ of banburying chamber's temperature, the pressure 0.2Mpa of banburying chamber, closed-smelting machine rotor rotating speed 1440r/min.
Preferably, aforesaid compounding process is: broken-(down)rubber is put into Banbury mixer, add vulcanization accelerator, vulcanization leveller, weighting agent, tackifying resin and sulphur more successively, mixing back banburying to plasticity number under 90~120 ℃ of conditions is 0.4~0.5.
The present invention also provides a kind of method of using sponge bonding to solve rubber overshoes sponge bubble: be pressed into together at the bottom of with sponge bonding and gelatin sponge by the sponge brush adhesive process, the compacting thickness of sponge bonding is 0.5~0.8mm, at the bottom of the gelatin sponge and the total thickness of sponge bonding be 2.8~3.6mm, carry out at the bottom of to the rubber gelatin sponge die-cut with 95~100 times/minute speed, then that the shiny surface of rubber overshoes outer bottom and the adhesive glue face orientation at the bottom of the rubber gelatin sponge is bonding, carry out pressing according to common process and cement.
Above-mentioned sponge brush adhesive process is: on roll 3 and in roll 4 backward rotation, drive sponge bonding 1 with in roll 4 roll in entering 4 and under roll between 5, simultaneously, in roll 4 and roll down at the bottom of the 5 backward rotation drive gelatin sponge 2, make 2 formation sponge composite gum compressed together at the bottom of sponge bonding 1 and the gelatin sponge; Rolling 4 temperature wherein and be 50 ℃~60 ℃, top roll and following roll temperature is 45~50 ℃, and the rotating speed of roller is 1440r/min.
Before carrying out the sponge brush adhesive process, it is even earlier sponge bonding to be refined soft refining, is rolled into the mixing packing element of diameter 10~15cm, length 40~45cm, can make easily like this sponge bonding tube by on roll 3 and in roll 4.
The present invention is that a large amount of experiments of having passed through the contriver draw, and is specific as follows:
One, sponge bonding prescription screening experiment
1, the calendering technology performance study of sponge bonding
Table 1 sponge bonding calendering technology performance test data
Test recipe number |
1# |
2# |
3# |
4# |
5# |
6# |
Rubber (part) |
100 |
100 |
100 |
100 |
100 |
100 |
Sulphur (part) |
2 |
2 |
2 |
2 |
2 |
2 |
Vulcanization accelerator (part) |
4 |
4 |
4 |
4 |
4 |
4 |
Vulcanization leveller (part) |
5 |
5 |
5 |
5 |
5 |
5 |
Weighting agent (part) |
185 |
185 |
185 |
170 |
185 |
200 |
Tackifying resin (part) |
30 |
45 |
55 |
45 |
45 |
45 |
Add up to (part) |
331 |
341 |
351 |
321 |
341 |
356 |
Gum content (%) |
30.21 |
29.33 |
28.49 |
31.15 |
29.33 |
28.09 |
The sponge bonding processing performance |
Glue is hard, the adhesive glue rubber is inhomogeneous, and the sponge bubble is arranged |
Technology is normal |
The adhesive glue roll banding is more serious |
The adhesive glue roll banding is more serious |
Technology is normal |
Glue is hard, the adhesive glue rubber is inhomogeneous, the sponge bubble is arranged and the sizing material scorching is arranged |
By above single factor simultaneous test, optimizing the tackifier consumption and be 45 parts, filler loading is 185 parts, carries out next step test based on this.
2. the sponge bonding vulcanization aid is to the influence of sponge bubble
(1) factor contrast
Table 2 factor synopsis
Annotate: other consumption of filling a prescription: rubber 100, weighting agent 185, tackifying resin 45.
(2) test arrangement (each test number is made 10 footwear)
Table 3 sponge bubble production rate
Test number |
1 |
2 |
3 |
4 |
5 |
6 |
7 |
8 |
9 |
Sulphur |
S1 |
S1 |
S1 |
S2 |
S2 |
S2 |
S3 |
S3 |
S3 |
Promotor |
A1 |
A2 |
A3 |
A2 |
A3 |
A1 |
A3 |
A1 |
A2 |
Promoting agent |
B2 |
B3 |
B1 |
B3 |
B2 |
B1 |
B1 |
B2 |
B3 |
Sponge bubble (only) |
5 |
4 |
5 |
0 |
0 |
5 |
4 |
3 |
0 |
Produce the frequency of sponge bubble:
S1=5+4+5=14;S2=0+0+5=5;S3=4+3+0=7
A1=5+5+3=13;A2=4+0+0=4;A3=5+0+4=9
B1=5+5+4=14;B2=5+0+3=8;B3=4+0+0=4
With regard to the aforementioned calculation result, filter out Cui prescription and be: S2, A2, B2; S2, A2, B3; S2, A3, B2; S2, A3, B3.
Through verification experimental verification, S2, A2, B2 are better than S2, A2, B3 and S2, A3, B3, and therefore preferred S2, A2, B2 are optimum consumption.Thereby the screening formulation of determining sponge bonding is: rubber 100, sulphur 2.5, vulcanization accelerator 5, vulcanization leveller 8, weighting agent 185, tackifying resin 45.
Two, rubber technology
The thickness of table 4 sponge bonding is to the influence of rubber overshoes quality (sponge bubble)
Sponge bonding thickness (mm) |
<0.30 |
0.40 |
0.50 |
0.60 |
0.70 |
Sponge bubble ratio (%) |
0.1~0.5 |
0.05 |
0.02 |
0.01 |
0.01 |
Sponge rises and sends out thickness (mm) |
8 |
7.5 |
7 |
7 |
6.5 |
Table 5 rubber gelatin sponge base thickness degree is to the influence of rubber overshoes quality (sponge bubble)
Rubber gelatin sponge base thickness degree (mm) |
2.8~3.0 |
3.1~3.2 |
3.3~3.5 |
3.6 |
3.7 |
Sponge bubble ratio (%) |
0 |
0 |
0.01 |
0.03 |
0.05 |
Sponge rises and sends out thickness (mm) |
5.5 |
6 |
6.8 |
8 |
8.5 |
Roll the influence of temperature and sponge bonding tube in table 6 rubber to the rubber effect
Roll in the rubber temperature (℃) |
<45 |
45~50 |
51~60 |
The sponge bonding surface |
Rubber is inhomogeneous |
Rubber is even |
Roll during sponge bonding is sticking |
Packing element diameter (cm) |
<10 |
12~15 |
>15 |
Result of use |
Frequently change glue |
Steadily |
Be difficult for into glue |
The storage time of table 7 adhesive glue
The storage time of adhesive glue (h) |
<0.5 |
0.5~1.5 |
>1.5 |
The sponge bonding surface |
Rubber is even |
Rubber is even |
Rubber is inhomogeneous |
Sponge bubble (%) |
0 |
0 |
0.05 |
Sponge thickness (mm) |
7 |
7 |
5.5~6.5 |
According to the data in table 4~7, the rubber thickness of selecting sponge bonding in the rubber technology be 0.5~0.7mm, rubber gelatin sponge base thickness degree 3.0~3.4mm, in to roll temperature be that 55 ℃, packing element diameter are 13~14cm.
Compared with prior art: (1) sponge bonding of the present invention has independently speed on curability, its sulfuration starting point is 1 minute 50 seconds~2 minutes and 20 seconds, guaranteed in just crosslinked typing in sponge foaming early stage, form one hardness height, insulating course that stress at definite elongation is high, stop gas expansion in the cavernous body to cause deformation layering at the bottom of rubber overshoes outer bottom and the gelatin sponge, suppress at the bottom of the gelatin sponge simultaneously and produce layering with the rubber overshoes outer bottom at the bottom of the gelatin sponge; (2) be bonded together securely at the bottom of rubber technology provided by the invention can make sponge bonding and gelatin sponge, avoid owing to the sponge that bottom slice produces at the bottom of the gelatin sponge and outside the rubber overshoes is steeped from technology; (3) sponge bonding of the present invention has enough viscosity, guarantees that sponge bonding and rubber overshoes outer bottom are bonded together well in rubber overshoes moulding production pressing process, has avoided producing layering between rubber overshoes outer bottom and the sponge bonding, thereby has eliminated the sponge bubble.The sponge bubble production rate of the rubber overshoes product after the present invention handles can reach below 0.03%, has significantly reduced the ratio of sponge bubble, has improved the quality of rubber overshoes.
Embodiment
Embodiment 1: take by weighing raw material in proportion: rubber 1000g, sulphur 25g, accelerator D S 50g, nano zine oxide (vulcanization leveller) 80g, potter's clay (weighting agent) 1850g and compound resin DS-B (tackifying resin) 450g.At first getting rubber plasticates in the XK-400 mill, 40~50 ℃ of machine roller temperatures, roll spacing 0.8mm, cross roll spacing 3~4 times, in the mill of roll spacing 9~10mm, rubber bag roll row is removed bubble then, make the plasticity number of rubber reach 0.45, promptly get broken-(down)rubber, then broken-(down)rubber is added Banbury mixer, add accelerator D S, nano zine oxide, potter's clay, compound resin DS-B more successively, mixing back banburying to plasticity number under 90~100 ℃ of conditions is 0.4~0.5, promptly gets sponge bonding.Test on the steam-heated vulcanizing press of 143 ± 1 ℃ of temperature, pressure 19.6Mpa, the sulfuration starting point of sponge bonding is 1 minute 50 seconds~2 minutes and 20 seconds.The sponge bonding of gained is refined soft refining in the XK-400 mill even, is rolled into the mixing packing element (margin is less than 12) of diameter 10~15cm, length 40~45cm.
Rubber technology: as shown in Figure 1, with mixing packing element is that sponge bonding 1 places and rolls 3 and roll between 4, on roll 3 and in roll 4 backscrollings, drive sponge bonding 1 with in roll 4 roll in entering 4 and under roll between 5, simultaneously, in roll 4 and roll down at the bottom of the 5 backscrollings drive gelatin sponge 2, make at the bottom of sponge bonding 1 and the gelatin sponge 2 compressed together.Rolling 4 temperature wherein and be 50 ℃~60 ℃, top roll and following roll temperature is 45~50 ℃.The compacting thickness of sponge bonding is 0.5~0.8mm, at the bottom of the gelatin sponge and the total thickness of sponge bonding be 2.8~3.6mm, carry out at the bottom of to the rubber gelatin sponge die-cut with 96 times/minute speed, then that the shiny surface of rubber overshoes outer bottom and the adhesive glue face orientation at the bottom of the rubber gelatin sponge is bonding, carrying out pressing according to common process cements, structure after bonding as shown in Figure 2, at the bottom of the gelatin sponge 2 and rubber overshoes outer bottom 6 between one deck sponge bonding 1 is arranged, after rubber technology, at the bottom of the gelatin sponge 2 and sponge bonding 1 in conjunction with firmly, avoided because the sponge that bottom slice produces at the bottom of the gelatin sponge and outside the rubber overshoes is steeped from technology.The sponge bubble production rate of the rubber overshoes product after the present invention handles can reach below 0.03%.
Embodiment 2: take by weighing raw material in proportion: rubber 800g, sulphur 20g, accelerator DM 60g, stearic acid (vulcanization leveller) 90g, potter's clay (weighting agent) 2100g and compound resin DS-B (tackifying resin) 400g, get the rubber 5~5.5min that on Banbury mixer, plasticates, the Banbury mixer condition is: 90~120 ℃ of banburying chamber's temperature, the pressure 0.2Mpa of banburying chamber, closed-smelting machine rotor rotating speed 1440r/min, make its plasticity number reach 0.4, add accelerator D S then successively, stearic acid, potter's clay, compound resin DS-B refines under 100~120 ℃ of conditions after mixing and promptly got sponge bonding in 4~6 minutes.
Rubber technology is as described in the embodiment 1.
Embodiment 3: take by weighing raw material in proportion: rubber 30kg, sulphur 0.75kg, accelerator DM 1.5kg, stearic acid (vulcanization leveller) 2.4kg, potter's clay (weighting agent) 55.5kg and compound resin DS-B (tackifying resin) 15kg, rubber plasticated make its plasticity number reach 0.5, add accelerator DM, stearic acid, potter's clay, compound resin DS-B then successively, mix the back and carry out the mixing sponge bonding that promptly gets according to common process.
Rubber technology is as described in the embodiment 1.