The art of improving plastics

This ability is an absolute necessity on markets with highly specialised requirements on plastics and composites.

The Brain resource makes it possible to develop innovative products while minimising the resulting production costs through consultation.

The Pigments resource is always tailored to customer specifications. Whether micronised or calcinated kaolin, fillers or colour silica sand for functional or aesthetic application.

There are no tricks to this art at bene_fit our specialist capability relies on controlled, solution-finding methodologies.

Comparison: Wet screen residue > 25 µm in calcined aminosilanised Kaolin

Several market known calcined aminosilanised kaolin types have been investigated. In each poduct the amount > 25 µm was analysed by wet screening.

bene_fit

 

Co_Nect PA KK 6, calcined kaolin, not silanised

 

Co_Nect PA KK 6_1_08, calcined kaolin, aminosilanised

Reference Products

  • 1 P
  • 2 N
  • 3 T

Wet Screen Residue > 25 µm

After dissolving the dry calcined kaolin in water the suspension has been wet screened using a 25 µm screen. The residue > 25 µm was dried and analysed. All tests have been carried out using an analytical screen, Fa. Retsch, 25 µm.
About 250 to 500 g of kaolin has been used to be dissolved in about 1-2 l destilled water. Additionally SEM-Pictures of each sample > 25 µm have been made.

Wet Screen residue > 25 µm

Material [mg/kg] Remark
Co_Nect PA KK 6 8,8  
Co-Nect PA KK 6_1_0
12,4  
1 P 1915  
2 N
57,6 Suspend in Butanol
3 T
897  

 

Result

The amount > 25 µm in the investigated samples is quite different. The bene_fit products do have the lowest value. The wet screen residue in the silanised calcined kaolin Co_Nect PA KK 6_1_08 is only slightly higher than in the unsilanised base kaolin Co_Nect PA KK.
The amount > 25 µm in the reference material is five to over 10 times higher.

Summary

From the tests can be seen, that the measurement of the wet screen residue > 25µm is an easy way to determine the coarse grain particles in calcined silanised
kaolin.
The results also show, that the bene_fit product Co_Nect PA KK 6_1_08 has the lowest wet screen residue in comparison to all investigated references.

Use of Elast_Al KK 60 in soft PVC blends - Stage 1

The Raw materials

Neralit 702 – PVC k=70, producer Spolana a.s. Neratovice
Naftosafe 2208 – Ca/Zn stabilizer , producer. Chemson Polymer Additive A.G.
DOP – Di-2-Ethylhexyl Phthalate, producer DEZA a.s. Valašké Mezirící
Elast_Al KK 60: calcined kaolin, producer bene _fit GmbH
Elast_Al KK 62_08: calcined kaolin, vinylsilanised, producer bene_fit GmbH
Omyacarb 2VA – calcium carbonate filler, producer Omya AG

Test sample preparation

The raw materials according table I except DOP were mixed on 1°high speed mixer at maximum speed up to 60°C. Than the first half of the DOP quantity was added, mixed up to 80°C and at least the second half of DOP was added, mixed up to 120°C, cooled down to 60°C at 100 rpm. The blend was granulated on PR-46, BUSS KO kneader at 125, 130, 125°C. The test samples were cut out from tables formed from folia in press at 170°C after 5 minutes preheating and 2 minutes of full pressure 300 bars. The folia was prepared on calander at 150°C 21 rpm, friction 1:1,4 after 3 minutes of preheating mixed for 5 minutes.

 

Sample No.
1 2 3 4 5 6
Component phr phr phr phr phr phr
Neralit 702 100 100 100 100 100 100
DOP 54 54 54 54 54 54
Naftosafe 2208 4,5 4,5 4,5 4,5 4,5 4,5
Elast AI KK 60       10 25  
Elast AI KK 62_08           10
Omyacarb 2VA   10 25      

 

Volume Resistance

Results

Some selected results are displayed in diagram 1. The results show that the volume resistance at both temperatures – room temperature and 70°C - is higher in the case of calcined kaolin than at the similar loadings of calcium carbonate even at 10 phr loading.
The processability of the blends was estimated by extrusion of 1x10mm band, without calibration, on single screw extruder (diameter 20mm, L/D=25, compression 1:2,5) at 140, 145, 150°C, melt temperature 161°C, screw speed 10, 20 and 40 rpm.
All the tested samples show the standard behaviour as a common soft PVC blend and there were no significant differences between all samples.
The Owen test shows that the used fillers do not affect thermal stability of the material.

Use of Elast_Al KK 60 in soft PVC blends - Stage 2

The Raw materials

Neralit 702 – PVC k=70, producer: Spolana a.s. Neratovice
Naftosafe 2208 – Ca/Zn stabilizer , producer: Chemson Polymer Additive A.G.
Naftosafe K 2011 – Ca/Zn stabilizer , producer: Chemson Polymer Additive A.G.
DOP – Di-2-Ethylhexyl Phthalate, producer: DEZA a.s. Valašké Mezirící
T.M.O.-L – trimelitate plasticizer, producer: EMSA CHEMICALS S.L.
Elast Al KK60 – calcined kaolin, producer: bene _fit GmbH
Elast Al KK62-08 – calcined kaolin, vinylsilanised, producer: bene _fit GmbH
Omyacarb 2VA – calcium carbonate filler, producer: Omya AG

Test sample preparation

The raw materials according to table 1 except Trimelitate were mixed on 1°high speed mixer at maximum speed up to 60°C and than the first half of the Trimelitate quantity was added, mixed up to 80°C. Than the second half of Trimelitate was added, mixed up to 120°C, cooled down to 60°C at 100 rpm.
The blend was granulated on PR-46, BUSS KO kneader at 125, 130, 125°C for blends with DOP or at 135, 140, 135°C for blends with Trimelitate.
The test samples were cut out from tables formed from folia in press at 170°C after 5 minutes preheating and 2 minutes of full pressure 300 bars.
The folia was prepared on calander at 150°C 21 rpm, friction 1:1,4 after 3 minutes of preheating mixed for 5 minutes.

 

Sample No.
1 2 3 4
Component phr phr phr phr
Neralit 702 100 100 100 100
Trimelitát T.M.O.-L 54 54 54 54
Naftosafe 2208 12 12 12 12
Elast AI KK 60   20 10  
Elast AI KK 62_08       20
Omyacarb 2VA 20   10  

 

Volume Resistance

Comparison of carbonate filler and nontreated/treated calcined kaolin

sample1 - carbonate filler 10phr
sample2 - nontreated calcinated kaolin 10phr
sample3 - treated calcined kaolin 10phr

Volume Resistance

Results

The results from selected tests are displayed in diagram 1 and 2.
The tests in stage 2 were focused on testing calcined kaolin in VDE0207 YI8 grade blend.
The results show that all types of fillers are able to fulfill the VDE0207 demand on YI8 grade.
Blends with calcined kaolin give better properties than the one with calcium carbonate filler. The blend with vinylsilanised calcined kaolin give the best or second best results in the major part of tests.
The vinylsilanised calcinated kaolin blend give generally the best results in the case of water treated samples.

Noncalcined and Calcined Kaolin in an EPDM-Recipe Recipe No 1

  • Specific processed waterwashed kaolin
    with or without surface treatment
    Base Kaoline
    Elast_Al K 45
    Elast_Al K 55
    Elast_Al K 80

 

 

 

 

  • Specific processed calcined kaolin
    with or without surface treatment
    Base Kaoline
    Elast_Al K 60
    Elast_Al K 80
    Elast_Al K 15 FD

 

 

 

 

 

 

Recipe 1 phr Step
Vistalon 7000 (Exxon) 100 phr 1
Silanogran HVS 2,45 phr 1
Filler (variable, 1-7) 130 phr 1
Omyalite 95T 90 phr 2
Struktol WB16 3 phr 2
Paraffine AW2152 7 phr 2
Mediaplast EPP/CON 43,65 phr 2
TMQ 1 phr 2
TAC-50% 4 phr 2
Perkadox 14/40Bpd 2 phr M
*) Reference
Filler Number
Calc. Kaolin 60 %<µm* 1
Elast_Al KK 60 2
Calc. Kaolin, 60 %<2µm, silan* 3
Elast_Al KK 62_08 4
Calc, 60 %<2µm* 5
Elast_Al K 45 6
Elast_Al K 80 7
*) Reference
Time (min) Step
Kneader (3) 1
Kneader (4) 2
Masticator M
 
Rheological Values
(175°C, 6 min; ISO 6502)
Calc
Kaolin
60%
<2µm*
Elast_Al
KK 60
Calc.
Kaolin,
60%
<2µm,
silan*
Elast_Al
KK 62_08
Kaolin,
60%
<2µm*
Elast_Al
K 45
Elast_Al
K 80
MI [dNm] 0,72 0,65 0,81 0,78 0,76 0,71 0,76
Mh [dNm] 9,7 8,9 10,55 10,33 8,96 10,67 9,14
t s2 [min] 1,58 1,69 1,51 1,49 1,36 1,21 1,31
T 90 [min] 5,11 5,11 5,09 5,05 4,93 4,98 4,98
               
Mechanical Values              
Hardness [°Sh A] ISO 868 73 72 73 73 73 77 76
Modulus 100 [MPa] ISO 37 2,4 2,5 2,8 3 2,8 3,5 4,5
Modulus 300 [MPa] 5,1 5,8 6,3 6,5 4,2 4,3 5,3
Tensle strength [MPa] 5,8 6,3 6,6 6,9 5,4 5,2 5,4
Elongation [%] 583 462 464 419 711 766 393
Tear resistance.[N] ISO 816 27,8 28,6 26,8 26,8 27,2 32,8 37
Impact elasticity [%] ISO 815;
24St.70°C
28,7 29,7 27,9 26,9 36,7 37,01 33,7
Stoßelastizität [%] ISO 4662 45 45 44 43 45 43 44
Abrasion [mm³] ISO 4649 495 432 448 437 505 547 412
Noncalcined and Calcined Kaolin in an EPDM-Recipe Recipe No 2

  • Specific processed waterwashed kaolin
    with or without surface treatment
    Base Kaoline
    Elast_Al K 45
    Elast_Al K 55
    Elast_Al K 80

 

 

 

 

  • Specific processed calcined kaolin
    with or without surface treatment
    Base Kaoline
    Elast_Al K 60
    Elast_Al K 80
    Elast_Al K 15 FD

 

 

 

 

 

 

Recipe phr Step
Keltan 5508 (DSM) 100 phr 1
Silanogran HVS 2,45 phr 1
Filler (variable, 1-2) 130 phr 1
Omyalite 95T 90 phr 2
Struktol WB16 3 phr 2
Paraffine AW2152 7 phr 2
Mediaplast EPP/CON 43,65 phr 2
TMQ 1 phr 2
TAC-50% 4 phr 2
Perkadox 14/40Bpd 2 phr M
 
Filler Number
Calc. Kaolin, 60 %<2µm, silan* 1
Elast_Al KK 62_08 2
*) Reference
Time (min) Step
Kneader (3) 1
Kneader (4) 2
Masticator M
 
Rheological Values, (175°C, 6 min; ISO 6502) Calc. Kaolin, 60 %<2µm, Silanised
Elast_Al KK 62_08
MI [dNm] 0,87 0,77
Mh [dNm] 10,56 9,97
t s2 [min] 1,45 1,44
T 90 [min] 5,06 5,03
     
Mechanical Values    
Hardness [°ShA] ISO 868 68 67
Modulus 100 [MPa] ISO 37 2,1 2,4
Modulus 300 [MPa] 5,1 5,5
Tensile strength [MPa] 5,6 5,9
Elasticity [%] 400 434
Tear strength [N] ISO 816 21,8 21,4
Compression elasticity [%] ISO 815; 24St.70°C 23,6 24,1
Impact elasticity [%] ISO 4662 41 43
Abrasion [mm³] ISO 4649 510 434
Noncalcined and Calcined Kaolin in a SBR-Recipe

  • Specific processed waterwashed kaolin
    with or without surface treatment
    Base Kaoline
    Elast_Al K 45
    Elast_Al K 55
    Elast_Al K 80

 

 

 

 

  • Specific processed calcined kaolin
    with or without surface treatment
    Base Kaoline
    Elast_Al K 60
    Elast_Al K 80
    Elast_Al K 15 FD

 

 

 

 

 

 

Recipe phr Step
Intol SBR 1502 40 phr 1
Eur. Neocis BR40 30 phr 1
Europrene H 865 30 phr 1
Struktol 60 NS 4,5 phr 2
Stearin acid 1 phr 2
PEG 4000 2 phr 2
Vulkanox 3010 1,5 phr 2
Silox HR 30 3 phr 2
Perkasil KS 408 GR 23 phr 2
Filler (variable 1- 6) 37 phr 2
CBS-80 % 2,8 phr M
MBT- 80% 1,25 phr M
Mixland S80 2,5 phr M
 
Filler Number
Kaolin 1* 1
Elast_Al KK 60 2
Calc. Kaolin. 50%<2µm* 3
Kaolin 2* 4
Elast_Al K 45 5
Elast_Al K 80 6
*) Reference
Time (min) Step
Kneader (3) 1
Kneader (4) 2
Masticator M
 
Rheological Values
(175°C, 6 min; ISO 6502)
Kaolin 1* Elast_Al K 45 Elast_Al K 80 Calc.
Kaolin.
50%<2µm*
Elast_Al
KK 60
Kaolin 2*
MI [dNm] 1,52 1,78 1,78 1,78 1,58 1,58
Mh [dNm] 15,87 16,97 16,23 18,46 17,24 14,65
t s2 [min] 1,17 1,08 1,04 1,21 1,22 1,19
T 90 [min] 2,23 2,11 2,04 2,36 2,33 2,21
             
Mechanical Values            
Hardness [°ShA] ISO 868 75 79 79 76 75 75
Modulus 100 [MPa] ISO 37 3 3,6 3,7 2,7 2,6 2,8
Modulus 300 [MPa] 6,6 7,1 7,3 6,1 6 5,6
Tensile Strength [MPa] 11,7 11,9 13,5 10,2 10,1 13,1
Elasticity [%] 477 465 509 456 461 535
Tear resistance [N] ISO 816 29,8 32,2 36 28 26,8 32,2
Compression elasticity [%] ISO 815;
24St.70°C
33,2 35,5 36,8 29,5 31,7 33,9
Impact elasticity [%] ISO 4662 40 38 38 40 40 37
Abrasion [mm³] ISO 4649 208 262 307 275 270 148
Functional Filler as a flame retardant in duroplastic polymers

Introduction

Polymers that are used in some specific applications have to have a well defined charcteristics regarding to their behaviour during burning. An example for that is a low flamability. As a rule, flame retarding mineral fillers like Mg(OH)2, ATH or organic additives are
used.
In a test procedure new high brightness mineral filler products are investigated with respect to their flame retarding activity. In addition, the mineral filler may improve the mechanical characteristics.

Project partner

Institute and own research

Methods

Standard methods for processing duroplastics

Functional Filler

VP FRF_1_G and VP FRF_1_D

Summary

  • The functional fillers were easily brought into the polymer.
  • Both materials were showing improvements in the mechanical stability
  • Also both functional fillers are showing a flame retarding activity in the polymer
Verbesserte mechanische Beständigkeit von Duroplasten durch Zusatz neuartiger Wirkstoffsysteme

Introduction

For duroplastic polymers a very high mechanical durability is required. This is also the case for duroplastics with very high filler loadings. In addition improvements in abrasion and scratch resistence are of special interest.
Tests are done to find out the advantages of new additive systems in mineral filled duroplastics.

Project partner

Institute, Pilotcustomer

Methods

Standard methods for processing duroplastics with high filler loading

Additive system

VP NFSI_1

Results

Improvements of the mechanical values, examples:

  • Modulus
  • Crackresistence
  • Elongation at break
  • Tensile Strength

Summary

  • Using the new additiv systems resulted in much improved mechanical values
  • Now the results and experiences are going to be transferred to other materials in new applications
  • Next step is the upscaling of the additiv systems within a prodution trial in cooperation with a pilotcustomer