CN103980540B - Rubber reinforcing filler and preparation method thereof - Google Patents

Abstract

A kind of rubber reinforcing filler, it comprises the formula of following percentage by weight: silane coupler 2%～4%, rare earth 0.5%～3.5%, all the other are tripoli. Preparation method is: 1), tripoli is calcined; 2), sorting, sorting standard is SiO₂>=95%; 3), mill, granularity requires as >=2000 orders; 4), add the silane coupler reaction time; 5), add rare earth reaction; 6), until step 5) in powder cooling after, powder is carried out to the filling finished product that is. Compared with prior art, it is simpler that the present invention has production technology, and the production cycle is relatively short, and production cost is lower, and reinforcement level can reach the reinforcement level of semi-reinforcing hydrocarbon black and add elasticity and the anti-rich good feature of property in the wrong of rear rubber.

Description

Rubber reinforcing filler and preparation method thereof

Technical field

The invention belongs to rubber filling material technology field, particularly relate to a kind of rubber reinforcing filler and preparation method thereof.

Background technology

In rubber, in order to reach different mechanical strengths, need to add rubber reinforcing filler at present. Conventionally be divided into two kinds,One is carbon black, and another kind is diatomite; Although and the former reinforcement level is better, production technology is more complicated, production processLoaded down with trivial details, production cost is higher; Although and the latter's production technology is simpler, production cost is relatively low, diatomite need throughCross natural dryingly, make the production cycle longer, and reinforcement level cannot reach the reinforcement level of semi-reinforcing hydrocarbon black, moreover after addingThe elasticity of rubber is relative poor with the anti-property of having mercy on of bending.

Summary of the invention

The present invention is directed to above problem provides a kind of production technology simpler, and the production cycle is relatively short, and production cost is lower, mendsStrong level can reach the reinforcement level of carbon black and add the elasticity of rear rubber and resist and bend the rich good rubber reinforcing filler of property.

The present invention overcomes the above problems technical scheme used: a kind of rubber reinforcing filler is provided, and it comprises following percentage by weightFormula:

Silane coupler 2%～4%, rare earth 0.5%～3.5%, all the other are tripoli.

Another object of the present invention is to provide a kind of preparation method of rubber reinforcing filler, and it comprises the following steps:

1), by tripoli calcining, calcining heat is 1000～1800 DEG C, the time is 1～6 hour;

2), to calcining after tripoli carry out sorting, sorting standard is SiO₂≥95％；

3), the tripoli after sorting put into airflow milling mill, granularity requires as >=2000 orders;

4), by step 3) powder that obtains puts into reactor, and adds 2%～4% silane coupler to stir, temperature is120～150 DEG C, the reaction time is 2～8 minutes, does not stop to stir;

5) in reactor, add, subsequently 0.5%～3.5% rare earth, temperature is 120～150 DEG C, and the reaction time is 10～20 minutes,Do not stop to stir;

6), until step 5) in powder cooling after, powder is carried out to the filling finished product that is.

Adopt after above formula and method, compared with prior art, although the present invention has added rare earth, the base-material using is siliconSoil, the cost of tripoli is relatively low, can significantly reduce costs; And add after rare earth, make the surface-active of powder better,Therefore rubber more can be adsorbed on powder surface well, absorption is a kind of physical process, i.e. attraction between powder and rubber moleculeBe greater than the cohesive force between rubber molecule; And mainly play strengthening action and be the inhomogeneities of powder, active very large work on powderChange point, have and there is no the electronics that matches, can play chemical action with rubber, have if rubber is adsorbed on the surface of powderDry point plays chemical combination with powder surface, and this effect can be described as chemisorbed, and chemisorbed is than simple physical absorptionMuch bigger, the feature of this chemisorbed is that strand ratio is easier to move on powder surface, but is difficult for and powder disengaging, thisSample rubber and powder have just formed a kind of strong key that can slippage, and this key has produced the effect of second reinforcement, and firstIndividual reinforcement effect is that the slippage of strand and a large amount of physisorptions can absorb in the time that rubber is subject to External Force Acting and is out of shapeThe impact of external force, the friction that external force is caused or hysteresis deformation play cushioning effect; Second effect is to make stress distribution even. ThisThe result of two effects makes that rubber is powerful to be increased, opposing is torn, and the elasticity that can too not damage again rubber simultaneously (is strandMotion), thus in the lower-cost while, also can significantly improve the mechanical and physical performance of rubber, make rubber processing stability,Elasticity, anti-rich, the anti-flammability etc. of bending are all better, and reinforcement level can reach the reinforcement level of semi-reinforcing hydrocarbon black; Simultaneously due to production workSkill is simpler, and after calcining, the production cycle is shorter, can significantly enhance productivity, and then reduce production costs. Therefore originallyIt is simpler that invention has production technology, and the production cycle is relatively short, and production cost is lower, and reinforcement level can reach semi-reinforcing hydrocarbon blackReinforcement level and add after rubber elasticity and anti-bend the rich good feature of property.

As preferably, described calcining heat is 1200～1800 DEG C, and the time is 2～6 hours.

As preferably, described silane coupler is Si-69 (chemical name is: two-[γ-(triethoxysilicane) propyl group] tetrasulfide).

Detailed description of the invention

Below in conjunction with specific embodiment, the present invention is described further.

Embodiment 1

A preparation method for rubber reinforcing filler, it comprises the following steps:

1), by tripoli calcining, calcining heat is 1000 DEG C, the time is 6 hours;

2), to calcining after tripoli carry out sorting, sorting standard is SiO₂≥95％；

3), the tripoli after sorting put into airflow milling mill, granularity requires as >=2000 orders;

4), by step 3) powder that obtains puts into reactor, and adds 4% silane coupler to stir, temperature is 120 DEG C,Reaction time is 8 minutes, does not stop to stir, and silane coupler is VTES;

5) in reactor, add, subsequently 3.5% rare earth, temperature is 120 DEG C, and the reaction time is 20 minutes, does not stop to stir;

6), until step 5) in powder cooling after, powder is carried out to the filling finished product that is.

Embodiment 2

A preparation method for rubber reinforcing filler, it comprises the following steps:

1), by tripoli calcining, calcining heat is 1200 DEG C, the time is 5 hours;

2), to calcining after tripoli carry out sorting, sorting standard is SiO₂≥95％；

3), the tripoli after sorting put into airflow milling mill, granularity requires as >=2000 orders;

4), by step 3) powder that obtains puts into reactor, and adds 3% silane coupler to stir, temperature is 140 DEG C,Reaction time is 6 minutes, does not stop to stir, and silane coupler is γ-methacryloxypropyl-trimethoxy silane;

5) in reactor, add, subsequently 3% rare earth, temperature is 140 DEG C, and the reaction time is 16 minutes, does not stop to stir;

6), until step 5) in powder cooling after, powder is carried out to the filling finished product that is.

Embodiment 3

A preparation method for rubber reinforcing filler, it comprises the following steps:

1), by tripoli calcining, calcining heat is 1500 DEG C, the time is 2 hours;

2), to calcining after tripoli carry out sorting, sorting standard is SiO₂≥95％；

3), the tripoli after sorting put into airflow milling mill, granularity requires as >=2000 orders;

4), by step 3) powder that obtains puts into reactor, and adds 2.5% silane coupler to stir, temperature is 130DEG C, the reaction time is 4 minutes, does not stop to stir, silane coupler is Si-69;

5) in reactor, add, subsequently 2% rare earth, temperature is 130 DEG C, and the reaction time is 15 minutes, does not stop to stir;

6), until step 5) in powder cooling after, powder is carried out to the filling finished product that is.

Embodiment 4

A preparation method for rubber reinforcing filler, it comprises the following steps:

1), by tripoli calcining, calcining heat is 1800 DEG C, the time is 1 hour;

2), to calcining after tripoli carry out sorting, sorting standard is SiO₂≥95％；

3), the tripoli after sorting put into airflow milling mill, granularity requires as >=2000 orders;

4), by step 3) powder that obtains puts into reactor, and adds 2% silane coupler to stir, temperature is 150 DEG C,Reaction time is 2 minutes, does not stop to stir, and silane coupler is Si-69;

5) in reactor, add, subsequently 0.5% rare earth, temperature is 150 DEG C, and the reaction time is 10 minutes, does not stop to stir;

6), until step 5) in powder cooling after, powder is carried out to the filling finished product that is.

Embodiment 5

A preparation method for rubber reinforcing filler, it comprises the following steps:

1), by tripoli calcining, calcining heat is 1800 DEG C, the time is 1～6 hour;

2), to calcining after tripoli carry out sorting, sorting standard is SiO₂≥95％；

3), the tripoli after sorting put into airflow milling mill, granularity requires as >=2000 orders;

4), by step 3) powder that obtains puts into reactor, and adds 4% silane coupler to stir, temperature is 150 DEG C,Reaction time is 8 minutes, does not stop to stir, and silane coupler is Si-69;

5) in reactor, add, subsequently 3% rare earth, temperature is 150 DEG C, and the reaction time is 20 minutes, does not stop to stir;

6), until step 5) in powder cooling after, powder is carried out to the filling finished product that is.

Above embodiment is only preferred embodiment of the present invention, and the present invention is not limited only to above embodiment and has also allowed other to change, allIn rights to independence claimed range of the present invention, change, all belong to protection domain of the present invention.

Claims (3)

1. a preparation method for rubber reinforcing filler, this rubber reinforcing filler comprises the formula of following percentage by weight: silane coupler2%～4%, rare earth 0.5%～3.5%, all the other are tripoli, it is characterized in that: it comprises the following steps:

1), by tripoli calcining, calcining heat is 1000～1800 DEG C, the time is 1～6 hour;

2), to calcining after tripoli carry out sorting, sorting standard is SiO₂≥95％；

3), the tripoli after sorting put into airflow milling mill, granularity requires as >=2000 orders;

4), by step 3) powder that obtains puts into reactor, and adds 2%～4% silane coupler to stir, temperature is120～150 DEG C, the reaction time is 2～8 minutes, does not stop to stir;

5) in reactor, add, subsequently 0.5%～3.5% rare earth, temperature is 120～150 DEG C, and the reaction time is 10～20 minutes,Do not stop to stir;

6), until step 5) in powder cooling after, powder is carried out to the filling finished product that is.

2. the preparation method of rubber reinforcing filler according to claim 1, is characterized in that: described calcining heat is1200～1800 DEG C, the time is 2～6 hours.

3. the preparation method of rubber reinforcing filler according to claim 1, is characterized in that: described silane coupler is Si-69.