CN1086740A - 以可吸性沉淀二氧化硅为基础的组合物 - Google Patents

以可吸性沉淀二氧化硅为基础的组合物 Download PDF

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CN1086740A
CN1086740A CN93106240A CN93106240A CN1086740A CN 1086740 A CN1086740 A CN 1086740A CN 93106240 A CN93106240 A CN 93106240A CN 93106240 A CN93106240 A CN 93106240A CN 1086740 A CN1086740 A CN 1086740A
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庞崇·杰安-路克
罗伯特·莱昂
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Rhodia Chimie SAS
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Abstract

本发明涉及以可吸性沉淀二氧化硅为基础的组 合物，其中本发明二氧化硅特点如下：BET表面至少 170m2/g；吸油量220—300ml/100g；压实态填充 密度至少0.29；平均粒径80—150mm；粒度分散指数 最大0.70且组合物中含有50—70wt％的液体，该组 合物密度高，流动性好且尘量低，尤其可用于补充人 畜饮食。

Description

本发明涉及以可吸性沉淀二氧化硅为基础的组合物。
众所周知可用二氧化硅载体载带液体，其目的是将不能或难于搬运的液体转化成易于包袋，例如成袋并可易于分散和混入其他细粒固体成分的流动粉。
所得组合物即二氧化硅载体吸收的液体下面称为载带组合物。
该组合物活性物质含量高且密度大，易搬运即流动性好且灰尘少。这些不同的要求有时是相抵触的。这些质量问题当然与用作载体的二氧化硅性质密切相关。
本发明第一目的是生产高质量可吸性二氧化硅。
本发明第二目的是制取高密度、高流动性和低尘量载带组合物。因此本发明可吸性沉淀二氧化硅特点如下：
BET表面至少170m2/g;
吸油量（DOP）220-300ml/100g;
压实态填充密度至少0.29;
平均粒径80-150mm;
粒度分散指数最大0.70。
已发现因上述特点的结合而使本发明二氧化硅特别适于作液体的载体。
当然，本发明还涉及以包括沉淀二氧化硅如上述二氧化硅载体吸收的液体为基础的载带组合物。
本发明其他特点和优点见下述及非限制性实例。
上述二氧化硅因上述性能组合而特别有用。
首先，该二氧化硅BET表面至少170m2/g，特别是至少210m2/g，优选为170-400m2/g或210-4003/g。
表面BET接Journal        of        American        Chemical        Society        vol，60，page309，February1938中所述BRUNAUER-EMMET-TELLER法和NF        T45007（5.11）标准测定。
本发明二氧化硅另一特点是其吸油量。吸油量（DOP）接NFT30-022（mars        53）标准测定，其中采用邻苯二甲酸二辛酯，吸油量为220-300ml/100g，特别是220-280且优选为240-280ml/100g。
其密度为至少0.29，为接AFNOR N0030100标准测定的压实态填充密度，特别是0.29-0.4且优选为0.29-0.36。
最后，粒度也为本发明二氧化硅的重要特点。
该粒度表明颗粒平均粒径d50为80-150mm，特别是90-130mm。
该粒度按NF        Ⅻ，507标准干性过筛测得。
此外本发明二氧化硅粒度分布很窄。这可由分散指数（I.D.）最大0.70，特别是0.6来加以说明。该指数对应于式（d84-d16）/2d50，其中dn表示直径，说明n%的颗粒粒径低于此直径值。
按本发明具体实施方案，二氧化硅还具有以下特点。
本发明二氧化硅一般pH4-8，特别是5.5-7。该PH按NFT-45007（5.5）测定。
另外，本发明二氧化硅优选为产品本身燃烧损失最多13%，而干产品为最多6%[NFT45007（5.3）]。
该二氧化硅可用多种方法制得如将硅酸盐与酸化剂反应，如与无机酸如碳酸，硫酸或盐酸反应。因此可将酸加入硅酸盐底部或同时将全部或部分酸和硅酸盐加入水桶底中，在盐或非盐或硅酸盐溶液存在下进行。
还可有利地进行处理，即在第一次沉淀后将硅酸盐溶液和/或酸引入反应介质中。
在反应糊过滤后，收集滤饼，必要时洗涤。滤饼然后一般粉化以进行干燥。
粉化时以及必要时在二氧化硅制法的各个先前步骤中，可有利地加入饼或在反应介质中加入呈低粘性或易泵送悬浮态的铝化合物。可参考FRN02536380。
优选条件是粉化态饼干燥前燃烧损失最多77%优选最多75%。
应注意到向饼中，特别是其粉化时加先期干燥的二氧化硅可得到该燃烧损失值。
干燥饼以得到最终产品的操作可按各种已知方式进行，如雾化，特别是用涡轮雾化器。
本发明二氧化硅特别适于载带液体，因此可制成载带组合物。
有大量液体可载带于载体上，如阴离子型洗涤用表面活性剂如磺酸盐或非离子型表面活性剂如醇或酚;橡胶业用硫化促进剂和抗氧化剂。
这里要特别提出补充人畜饮食的液体。
特别是维生素A，B，C，D，E和K。
维生素B中可特地举出胆碱和其衍生物，特别是胆碱盐酸盐。
二氧化硅载体吸收液体可按已知方式进行，如在混合器中将液体喷到二氧化硅上。
液体吸收量与用途有关。本发明二氧化硅可制成液体含量超过50%（重），特别是高达70%如50-60%的组合物。
一般，本发明二氧化硅可制成高密度，高流动性和低粉尘组合物。
具体如维生素，特别是维生素E和胆碱盐酸盐的组合物，其DRT至少0.60，特别是至少0.65，甚至至少0.70。
组合物倾斜角（按NFT20-221）为最高32°。
同一组合物的粉尘指数低于2，甚至低于1。
粉尘测定用法国专利申请8703159所述装置进行。
该装置连接到恒定微流装置上，将光电膜停留时间变化转化为拉伸状态，再于1-100mv梯度的电光表上以峰谷形式图示。峰的mV值为粉尘指数（IP）。
比较起来，同一组合物但用先前二氧化硅载体的IP至少为3。
维生素载带组合物的如前述分散指数最大0.55。
下述具体实例说明本发明。
实例1
该例制取本发明可吸性二氧化硅。
于70℃以比例3.5在硅酸钠桶底加硫酸。形成二氧化硅糊pH调为5后过滤并将湿滤饼洗涤后粉化。
粉化时加入先期干燥的二氧化硅以使粉化滤饼的燃烧损失达75%。pH然后调为6.0。
粉化滤饼喷雾干燥后得特点如下的二氧化硅：
pH        6.7        DOP        250ml/100g
DRT 0.32 BET 270m2/g
D50105um ID 0.5
实例2
用实例1二氧化硅作维生素E的载体。
在以20T/mn转动并且其内轴以1900T/mn转动的71V型混合器中将维生素载于载体上，其中横向装有板，借此将维生素喷雾并将滚刀固定在其上。
将上述二氧化硅全部加入混合器后再将维生素喷到二氧化硅上，混合5分钟后再均化2分钟。
维生素固持温度70℃，恒定流量100ml/mn。
最终混合物中，重量比为46%SiO2和54%d，1-α生育粉的乙酸盐。
组合物特点如下：
DRT        0.70        倾角        30°
d5090um ID<1
ID        0.55
实例3
该例制取第二种本发明可吸性二氧化硅。
操作同实例1。不过，反应后再多一次处理，其中向反应介质中引入硫酸钠溶液和硫酸。
洗涤并粉化滤饼后加先期干燥的二氧化硅，以达到74%的粉化饼的燃烧损失。还向饼中加易泵送粉化悬浮液态的铝酸钠（4000ppm（重），以无水二氧化硅计）。pH调为6并且悬浮液同实例1干燥。
所得二氧化硅特点如下：
pH 7.0 ID 0.5 d50100um
DRT 0.34 DOP 240ml/100g BET 200m2/g
实例4
操作同实例2，但将胆碱盐酸盐载带于实例3二氧化硅上。
最终组合物中比例如下：60份（重）70%胆碱盐酸盐水溶液，40份二氧化硅，0.3份添加剂（硬脂酸镁）。
组合物特点如下：
DRT        0.77        IP        1.6
倾角        31°        ID        0.5
d5090um
实例5比较
用RHONE-POULENC公司以商标Tix-O-Sil38A销售的二氧化硅作载体，其特点如下：
pH        7        ID        >0.7
DRT        0.22        DOP        340ml/100g
d5060um BET 330m2/g
在与实例2相同条件下以维生素E为基础的组合物特点如下：
DRT        0.50        倾角        41°        ID>0.7
d5080um IP >5
可以看出，与实例1比较，该组合物流动性低且粉尘量大。

Claims (6)

1、载带组合物，其特征在于其中包括用特点如下的沉淀二氧化硅载体吸收的液体：
BET表面至少170m2/g。
吸油量(DOP)220-300ml/100g。
压实态填充密度至少0.29；
粒度分散指数最大0.70；
该组合物中液体含量50-70wt%。
2、根据权利要求1所述的组合物，其特征在于二氧化硅BET表面至少210m2/g，特别是210-400m2/g。
3、根据权利要求1所述的组合物，其特征在于二氧化硅吸油量220-280ml/100g。
4、根据权利要求1-3之一所述的组合物，其特征在于二氧化硅pH4-8。
5、根据权利要求1所述的组合物，其特征在于其压实态填充密度至少0.60，特别是至少0.65。
6、根据权利要求1所述的组合物，其特征在于其倾角最大32°。
CN93106240A 1988-05-19 1993-05-24 以可吸性沉淀二氧化硅为基础的组合物 Expired - Fee Related CN1034557C (zh)

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CN1758901B (zh) * 2003-02-19 2010-04-28 生命周期药物公司 硅石或硅石衍生物作为吸附材料的用途

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FR2631620A1 (fr) 1989-11-24
TR23943A (tr) 1990-12-21
JPH055768B2 (zh) 1993-01-25
KR940009929B1 (ko) 1994-10-19
ES2058568T3 (es) 1994-11-01
US5635214A (en) 1997-06-03
NO891989D0 (no) 1989-05-18
ZA893716B (en) 1991-04-24
FR2631620B1 (fr) 1990-07-27
EP0345109A1 (fr) 1989-12-06
DE68909113D1 (de) 1993-10-21
YU101589A (en) 1991-02-28
HUT50724A (en) 1990-03-28
JPH0244023A (ja) 1990-02-14
DK175708B1 (da) 2005-01-24
RU1836290C (ru) 1993-08-23
NO891989L (no) 1989-11-20
HU207968B (en) 1993-07-28
CN1034557C (zh) 1997-04-16
ATE94511T1 (de) 1993-10-15
DK240589A (da) 1989-11-20
AU3496789A (en) 1989-11-23
KR890017174A (ko) 1989-12-15
CN1042132A (zh) 1990-05-16
DE68909113T2 (de) 1994-03-17
BR8902688A (pt) 1990-01-23
IL90307A0 (en) 1989-12-15
NZ229162A (en) 1991-02-26
YU47018B (sh) 1994-11-15
CN1023788C (zh) 1994-02-16
FI892410A0 (fi) 1989-05-18
EP0345109B1 (fr) 1993-09-15
CA1340820C (fr) 1999-11-16
FI892410A (fi) 1989-11-20
DK240589D0 (da) 1989-05-18

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